CN114272159B - Washing liquid based on modified chitosan micro-nano fiber particles - Google Patents
Washing liquid based on modified chitosan micro-nano fiber particles Download PDFInfo
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Abstract
The invention provides a washing liquid based on modified chitosan micro-nano fiber particles, which comprises 0.1-3wt% of polydopamine, carboxylated modified chitosan nano fiber particles, a complexing agent, a thickening agent, a humectant, functional active components and the like. Wherein, the grafting amount of carboxyl on the polydopamine and carboxylation modified chitosan nano fiber particles is sequentially reduced from outside to inside of the fiber, so that the washing liquid is swelled but not dissolved during washing, and the softness and the elasticity are improved. The carboxyl on the surfaces of the polydopamine and carboxylation modified chitosan nanofiber particles has high hydrophilicity, so that the capacity of swelling the micro-nanofiber particles to form gel particles can be given, and the gel strength of the gel particles formed after imbibition can be improved by the polydopamine on the surfaces, so that dissolution is avoided; the surface of the fiber particle is also provided with positively charged amino groups, so that the micro-nano fiber particle can be endowed with good antibacterial performance. The washing liquid provided by the invention has remarkable friction washing effect and washing experience, and has good application prospect.
Description
Technical Field
The invention relates to the technical field of preparation of human body care cleaning agents, in particular to a washing liquid based on modified chitosan micro-nano fiber particles.
Background
Gynecological diseases such as colpitis, cervicitis, cervical erosion, etc., are easy to show symptoms of itching, peculiar smell, abnormal leucorrhea, burning lower body, etc. The occurrence of gynecological inflammation is closely related to the constitution and living habit of the women, the pathogenesis causes are complex and various, the female is hidden, and the living quality and family harmony of people are seriously affected. At present, more washing liquid for treating gynecological diseases mainly comprises two major types of traditional Chinese medicine lotion and western medicine lotion, but both lotions have respective defects, such as weaker traditional Chinese medicine lotion drug efficacy and long treatment time, and western medicine lotion has fewer drug components, single action and easy irritation, and the traditional Chinese medicine lotion and the western medicine lotion have the defects of easy recurrence after stopping drug withdrawal and longer treatment course.
Most of the existing washing liquid in the market at present does not contain an abrasive, and the refractory dirt hidden in private parts cannot be thoroughly cleaned; in addition, most private parts washing solutions also contain powerful bactericidal components, such as Chinese patent publication No. CN103263525A, publication No. 2013 and 28 months, the formula of the washing solution disclosed by the invention named as gynecological washing solution and a preparation method thereof contains high-concentration Chinese herbal medicine extracting solution, chinese patent publication No. CN103446177A, publication No. 2013 and 12 months and 18 days, and the formula of the washing solution disclosed by the invention named as the washing solution for treating gynecological diseases and the preparation method thereof contains chlorhexidine. The medicines such as the high-efficiency bactericidal components are easy to cause dependence on medicines for long-term use, destroy the balance of natural flora at private parts, interfere the self-cleaning capability of the private parts, and cause certain irritation to tender skin at the private parts, thereby having certain side effects.
Patent CN1823813a discloses a female vaginal care therapeutic composition, which solves the problem of drug resistance by utilizing the antibacterial property and biocompatibility of chitosan or cationic derivatives thereof. However, the still soluble cleaning solution used in this patent is still not satisfactory in cleaning effect. However, when the cleaning liquid is used for cleaning a human body, the friction injury of the friction agent to the human body is considered, and the friction agent is rarely added into the cleaning liquid for human body care in the prior art.
In view of the foregoing, there is a need for an improved washing solution based on modified chitosan micro-nanofiber particles to solve the above-mentioned problems.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a washing liquid based on modified chitosan micro-nano fiber particles, which improves the softness, elasticity and wear resistance of the fiber particles in the washing liquid by modifying carboxyl groups and dopamine of the chitosan fiber particles, thereby improving the friction washing effect and reducing the friction pain.
In order to achieve the aim of the invention, the invention provides a washing liquid based on modified chitosan micro-nano fiber particles, which comprises 0.1 to 3 weight percent of polydopamine and carboxylated modified chitosan nano fiber particles, wherein the grafting amount of carboxyl on the polydopamine and carboxylated modified chitosan nano fiber particles is sequentially reduced from outside to inside of the fiber, so that the washing liquid based on modified chitosan micro-nano fiber particles is swelled but not dissolved during washing, and the softness and the elasticity are improved.
As a further improvement of the invention, the preparation method of the polydopamine and carboxylated modified chitosan nanofiber particles comprises the following steps:
s1, crushing chitosan nanofiber obtained by spinning to obtain chitosan nanofiber particles with the diameter of 0.5-500 mu m and the length of 0.5-500 mu m;
s2, carrying out carboxylation grafting reaction on the chitosan nanofiber particles obtained in the step S1 in a solution with the ethanol volume content of more than 80%, so as to obtain carboxylated chitosan nanofiber particles, wherein the carboxyl grafting amount is sequentially reduced from the outside to the inside of the fiber;
s3, adding the carboxylated chitosan nanofiber particles obtained in the step S2 into a mixed solution of ethanol and water, and then adding dopamine hydrochloride to carry out a grafting reaction to obtain dopamine and carboxylated modified chitosan nanofiber particles;
s4, oxidizing and polymerizing the dopamine and carboxylated modified chitosan nanofiber particles obtained in the step S3 in a sodium periodate solution to obtain the polydopamine and carboxylated modified chitosan nanofiber particles.
As a further improvement of the present invention, in step S2, the carboxylation grafting reaction employs acrylic acid grafting, and the molar ratio of acrylic acid to chitosan nanofiber particles is 1:0.1 to 20.
As a further improvement of the invention, in the step S2, after the carboxylation grafting reaction is completed, the alkali washing is carried out by adopting a mixed solution of ethanol and water of sodium hydroxide, and then the washing is carried out to neutrality by adopting a mixed solution of absolute ethanol and deionized water.
As a further improvement of the invention, in the step S3, the volume ratio of the ethanol to the water is 4:1, and an NHS/EDC (N-hydroxysuccinimide/(1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride)) catalyst is also added into the mixed solution.
As a further improvement of the present invention, in step S3, the amino group on the dopamine hydrochloride reacts with the carboxyl group on the carboxylated chitosan nanofiber particle, and after the reaction is completed, the substitution degree of the carboxyl group is 0.2-0.3, and the substitution degree of the dopamine is 0.4-0.6.
As a further improvement of the present invention, in step S4, the time of the oxidative polymerization reaction is 10 to 20 hours; after the reaction is completed, the mixture is filtered, washed by ethanol and water in a volume ratio of 4:1 and dried.
As a further improvement of the invention, the washing liquid based on the modified chitosan micro-nano fiber particles comprises the following components in percentage by mass:
0.1 to 3 percent of polydopamine and carboxylated modified chitosan nanofiber particles;
5.0 to 25.0 percent of surfactant;
0.1 to 10 percent of humectant;
0.1 to 3.0 percent of thickening agent;
0.5 to 1.5 percent of conditioner;
0.1 to 0.3 percent of acidity regulator;
0.1 to 0.5 percent of preservative;
0.5 to 1.5 percent of solubilizer;
0.1 to 5.0 percent of functional active ingredient;
complexing agent 0.01-0.2%;
0.05 to 1.0 percent of essence;
92.84 to 49.0 percent of purified water.
As a further improvement of the invention, the surfactant is one or more of cocamidopropyl betaine, sodium fatty alcohol sulfate, ammonium dodecyl sulfate, sodium lauroyl glutamate, sodium lauroyl sarcosinate, cocoyl glutamate, fatty alcohol polyoxyethylene ether ammonium sulfate, disodium cocoyl amphodiacetate, disodium laureth sulfosuccinate, cocoyl hydroxysulfobetaine, alkyl glucoside, sodium cocoyl taurate, ammonium laurylsulfate, sodium myristoyl sarcosinate, sodium fatty alcohol polyoxyethylene ether sulfate, cocoyl monoethanolamine and sodium fatty acid methyl sulfonate;
the thickening agent is one or more of PEG-150 pentaerythritol tetrastearate, polyacrylic acid copolymer and sodium chloride;
the humectant is one or more of propylene glycol, glycerol, butanediol, sorbitol, amino acid humectant, trehalose, sodium hyaluronate, sodium polyglutamate and polyglycerol-10;
the acidity regulator is one or more of lactic acid and citric acid;
the preservative is one or more of potassium sorbate, sodium benzoate, triclosan, MIT (methyl isothiazolinone), cetylpyridinium chloride, chlorpheniramine, p-hydroxyacetophenone, phenoxyethanol, benzalkonium chloride, benzalkonium bromide, bromothalol, pinocele and 2, 4-dichlorobenzene alcohol;
the solubilizer is one or more of PEG-40 hydrogenated castor oil, laureth-7/laureth-9 and PEG-80 sorbitan laurate;
the functional active ingredients are one or more of ginseng extract, dipotassium glycyrrhizinate, hydrolyzed collagen, chitin, tea tree oil, menthol, borneol, aloe extract, honeysuckle extract, wild chrysanthemum extract, gingko extract, pearl hydrolysate, rose hydrosol, safflower extract, angelica extract, dandelion extract, papaya extract, tree peony root bark extract, acid bean seed extract and seaweed active peptide;
the stability is one or two of disodium ethylenediamine tetraacetate (EDTA disodium) and tetrasodium ethylenediamine tetraacetate (EDTA tetrasodium).
As a further improvement of the invention, the preparation method of the washing liquid based on the modified chitosan micro-nano fiber particles comprises the following steps: adding the complexing agent into purified water, stirring until the complexing agent is completely dissolved, heating to 60-80 ℃, sequentially adding the surfactant, the humectant and the conditioner, stirring uniformly, cooling to 55-40 ℃, sequentially adding the preservative, the functional active ingredient, the polydopamine, the carboxylated modified chitosan nanofiber particles, the thickener, the solubilizer, the essence and the acidity regulator, and stirring uniformly to obtain the washing liquid based on the modified chitosan micro-nanofiber particles.
The beneficial effects of the invention are as follows:
the washing liquid based on the modified chitosan micro-nano fiber particles provided by the invention adopts the chitosan nano fiber particles which have high specific surface area and high biocompatibility, and the surface roughness of the fibers is relatively high, so that the friction cleaning effect is good. After the polydopamine and the carboxyl are simultaneously modified, on one hand, the catechol groups of the carboxyl and the dopamine are utilized to improve the affinity to dirt, and certain objects to be cleaned can be removed through hydrogen bonds or complexation; on the other hand, the polydopamine is oxidized and crosslinked, so that the strength of chitosan fiber particles is improved, the chitosan fiber particles are swelled in water and are not dissolved, the wear resistance is good, and the chitosan fiber particles can be repeatedly rubbed and used without cracking; the softness and elasticity of the swollen fiber particles are improved, the friction comfort level is improved, and the harm to human bodies is reduced. The chitosan gel particles in the lotion can repeatedly rub with the deep layers of skin pores, so that tiny dirt is peeled off from the deep layers of the pores, and the micro emulsion is formed through the emulsification of the surfactant, so that the micro emulsion is removed to the skin surface, and the effect of thoroughly cleaning is achieved. Therefore, the cleaning liquid provided by the invention has remarkable cleaning effect and cleaning experience and good application prospect.
Drawings
FIG. 1 is a schematic structural diagram of polydopamine and carboxylated modified chitosan nanofiber particles prepared by the method.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail with reference to specific embodiments.
It should be further noted that, in order to avoid obscuring the present invention due to unnecessary details, only structures and/or processing steps closely related to aspects of the present invention are shown in the specific embodiments, and other details not greatly related to the present invention are omitted.
In addition, it should be further noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
The washing liquid based on the modified chitosan micro-nanofiber particles comprises 0.1-3wt% of polydopamine and carboxylated modified chitosan nanofiber particles, and the carboxyl grafting amount on the polydopamine and carboxylated modified chitosan nanofiber particles is sequentially reduced from outside to inside of the fiber, so that the washing liquid based on the modified chitosan micro-nanofiber particles is swelled but not dissolved during washing, and the softness and the elasticity are improved. In this way, the chitosan nanofiber particles adopted have high specific surface area and high biocompatibility, and the surface roughness of the fibers is relatively high, so that the friction cleaning effect is good. After the polydopamine and the carboxyl are simultaneously modified, on one hand, the catechol groups of the carboxyl and the dopamine are utilized to improve the affinity to dirt, and certain objects to be cleaned can be removed through hydrogen bonds or complexation; on the other hand, the polydopamine is oxidized and crosslinked, so that the strength of chitosan fiber particles is improved, the chitosan fiber particles are swelled in water and are not dissolved, the wear resistance is good, and the chitosan fiber particles can be repeatedly rubbed and used without cracking; the softness and elasticity of the swollen fiber particles are improved, the friction comfort level is improved, and the harm to human bodies is reduced. Therefore, the cleaning liquid provided by the invention has remarkable cleaning effect and cleaning experience and good application prospect.
The preparation method of the polydopamine and carboxylation modified chitosan nanofiber particle comprises the following steps:
s1, crushing chitosan nanofiber obtained by spinning to obtain chitosan nanofiber particles with the diameter of 0.5-500 mu m and the length of 0.5-500 mu m; the chitosan material had a degree of deacetylation of about 1.
S2, carrying out carboxylation grafting reaction on the chitosan nanofiber particles obtained in the step S1 in a solution (preferably ethanol) with the ethanol volume content of more than 80%, so as to obtain carboxylated chitosan nanofiber particles, wherein the carboxyl grafting amount is sequentially reduced from the outside to the inside of the fiber; the carboxylation grafting reaction is preferably acrylic acid grafting, and the molar ratio of acrylic acid to chitosan nanofiber particles is 1:0.1 to 20, preferably 0.8 to 3, more preferably 1 to 2; the substitution degree of carboxyl is 0.7-0.8, calculated according to the original amino content of substituted amino. In the step, the chitosan nanofiber particles are insoluble in ethanol, so that the molecular chain extension degree of chitosan is limited, acrylic acid is mainly grafted on the surface layer, and the grafting substitution degree inside the fiber is ensured to be less than 0.2 by controlling the reaction time. By doing so, the solubility of the nanofiber particles during cleaning can be reduced, and the friction cleaning effect can be prevented from being lost due to dissolution. The small internal substitution degree can keep the skeleton structure of the nanofiber particles, so that the nanofiber particles can absorb water and swell to form high-flexibility particles.
S3, adding the carboxylated chitosan nanofiber particles obtained in the step S2 into a mixed solution of ethanol and water, and then adding dopamine hydrochloride to carry out a grafting reaction to obtain dopamine and carboxylated modified chitosan nanofiber particles; referring to fig. 1, the amino groups of the dopamine hydrochloride and the carboxyl groups undergo amidation grafting reaction, so that part of the carboxyl groups are further substituted by the dopamine hydrochloride, the substitution degree of the carboxyl groups is 0.2-0.3, and the substitution degree of the dopamine is 0.4-0.6 after the reaction is completed.
S4, oxidizing and polymerizing the dopamine and carboxylated modified chitosan nanofiber particles obtained in the step S3 in a sodium periodate solution to obtain polydopamine and carboxylated modified chitosan nanofiber particles. The dopamine is oxidized and crosslinked under the action of sodium periodate, so that the strength of chitosan fiber particles is further improved, and after the chitosan gel particles are contacted with water, the liquid absorption swelling becomes soft and elastic gel particles with certain strength. When the lotion is applied to skin, chitosan gel particles in the lotion can repeatedly rub with deep pores of the skin, tiny dirt of the chitosan gel particles is peeled off from the deep pores, and microemulsion is formed through emulsification of the surfactant, so that the chitosan gel particles are removed to the surface of the skin, and the effect of thoroughly cleaning is achieved. In addition, the chitosan gel particles are soft and elastic, and can play a certain massage effect on the skin of private parts during cleaning, so that the feeling of tarnishing and pain caused by friction can be avoided.
Examples 1 to 3
The washing solutions based on modified chitosan micro-nanofiber particles provided in examples 1-3 have the components shown in Table 1.
The preparation method comprises the following steps: adding the complexing agent into the purified water according to the mass percentage, stirring until the complexing agent is completely dissolved, heating to 60-80 ℃, sequentially adding the surfactant, the humectant and the conditioner, uniformly stirring, cooling to 55-40 ℃, sequentially adding the preservative, the functional active ingredient, the polydopamine, the carboxylated modified chitosan nanofiber particles, the thickener, the solubilizer, the essence and the acidity regulator, and uniformly stirring to obtain the washing liquid based on the modified chitosan micro-nanofiber particles.
The preparation method of the polydopamine and carboxylation modified chitosan nanofiber particles comprises the following steps:
(1) The diameter of the chitosan micro-nano fiber particles is 20 mu m, the length is 80 mu m, and the chitosan micro-nano fiber particles are prepared by crushing chitosan nano fibers after spinning;
(2) Dispersing chitosan micro-nano fiber particles in ethanol, wherein the mass volume ratio of the chitosan micro-nano fiber particles to the ethanol is 1g:30mL, adding acrylic acid into the mixed solution of the chitosan micro-nano fiber particles and ethanol, wherein the molar ratio of the acrylic acid to the amino groups of the chitosan micro-nano fiber particles is 1:1.5, after stirring uniformly at room temperature, heating to 40-60 ℃ and reacting in a constant-temperature water bath for 4-48 h. After the reaction is finished, filtering, and alkali washing carboxylated chitosan micro-nano fiber particles with alkali liquor prepared by sodium hydroxide (wherein the alkali liquor is prepared by dissolving 32g of sodium hydroxide in 800ml of deionized water, adding 3400ml of absolute ethyl alcohol, namely, the alkali liquor is prepared by 4% sodium hydroxide and absolute ethyl alcohol in a volume ratio of 4:17) to be strong alkaline; then washing the carboxyl chitosan micro-nano fiber particles subjected to alkali washing to be nearly neutral by using a mixed solution of absolute ethyl alcohol/deionized water (volume ratio is 4:1), and washing for 3 times by using absolute ethyl alcohol; finally, drying in a drying oven at 50 ℃ to obtain carboxyl chitosan micro-nano fiber particles with the carboxyl substitution degree of 0.7-0.8;
(3) Adding dopamine hydrochloride into carboxyl chitosan micro-nanofiber particles with the carboxyl substitution degree of 0.7-0.8 in ethanol/water (volume ratio of 4:1), reacting for 24 hours at room temperature under the catalysis of NHS/EDC, filtering after the reaction is finished, washing with ethanol/water (volume ratio of 4:1), and drying to obtain the chitosan micro-nanofiber particles grafted with dopamine groups and carboxyl, wherein the carboxyl substitution degree is 0.2-0.3, and the dopamine substitution degree is 0.4-0.6;
(4) Dispersing the chitosan micro-nano fiber particles grafted with dopamine groups and carboxyl groups in water (solid-to-liquid ratio is 1:50), adding 5% sodium periodate solution, and reacting for 12 hours at room temperature. After the reaction is completed, filtering, washing with ethanol/water (volume ratio of 4:1), and drying to obtain the carboxyl chitosan@polydopamine (CECS@Poly Dopa) micro-nano fiber particles.
TABLE 1 the composition ratios of examples 1-3
Comparative example 1
The difference compared to example 1 is that polydopamine and carboxylated modified chitosan nanofiber particles are replaced with unmodified chitosan nanofiber particles. The other points are substantially the same as those of embodiment 1, and will not be described here again.
Comparative example 2
The difference compared to example 1 is that polydopamine and carboxylated modified chitosan nanofiber particles are replaced with carboxylated modified chitosan nanofiber particles, i.e. steps (3) and (4) of example 1 are removed. The other points are substantially the same as those of embodiment 1, and will not be described here again.
Comparative example 3
The difference compared to example 1 is that the polydopamine and carboxylated modified chitosan nanofiber particles are replaced with dopamine modified chitosan nanofiber particles, i.e. step (2) of example 1 is removed, and the polydopamine is adhered to the chitosan fiber surface in a physically coated form. The other points are substantially the same as those of embodiment 1, and will not be described here again.
Comparative example 4
The difference compared with example 1 is that the chitosan is carboxylated and then spun, and then the dopamine modification of steps (3) and (4) is carried out, wherein the carboxylation degree of the inner surface and the outer surface of the fiber is basically the same. The other points are substantially the same as those of embodiment 1, and will not be described here again.
The lotions of examples 1-3 and comparative examples 1-4 were subjected to a vaginal cleansing efficacy test, a skin-friendly test and an abrasion resistance test.
(1) Vaginal cleaning efficacy test: the gynecological cleaning solution is directly poured into a vaginal douche, then is inserted into a vaginal extrusion bottle body for washing, and is washed 2 times per day for 2-3 min each time, and the treatment effect is evaluated after a treatment course by taking 5 continuous days as a treatment course.
Treatment efficacy judgment
And (3) healing: subjective symptoms disappear, the vagina cleanliness (I), the vagina swab is cultured to turn into yin, and the repeated examination after 4 times of menstruation is negative;
the method is effective: subjective symptoms are relieved, the vaginal cleanliness (II) is achieved, the vaginal swab is cultured to grow only a few bacteria, and even trichomonas or mould is seen, the number of the bacteria is not more than 10 at most, and the patients with positive symptoms are rechecked for 2 times after 4 times of menstruation; the total recovery and effective sum is the total effective rate.
Invalidation: no improvement in subjective symptoms, no change in vaginal cleanliness, and no change in vaginal swab culture.
The test results are shown in Table 2, in which the test group is example 1 and the control group is the washes of comparative examples 1 to 4, respectively.
TABLE 2 cleaning efficacy test results
From Table 2, it can be seen that the chitosan fiber particles modified by the invention have better cleaning effect on both mycotic vaginitis and bacterial vaginitis. And the chitosan fiber particles are basically harmless to the skin, have good cleaning experience and can realize deep cleaning by combining the test of the swelling breaking rate. The unmodified chitosan fiber particles are adopted, so that the cleaning effect is remarkably reduced, and the unmodified chitosan fiber particles cannot be swelled to form gel, so that the flexible friction effect is poor. The carboxyl-modified chitosan fiber particles alone were improved compared to the unmodified ones, but were still lower than in example 1 because of lower strength, easy breakage during washing, resulting in reduced friction washing effect. The dopamine-modified chitosan fiber particles alone have a higher cleaning effect than unmodified and lower than carboxyl, and as can be seen from the test results in table 3, the dopamine-modified chitosan fiber particles alone have an improved strength by crosslinking, but are difficult to absorb water and swell to form gel, so that the friction cleaning effect is poor.
(2) Skin affinity test: test and control groups were established, each group of 10 adult healthy SD rats.
Test group: after the cotton sliver is immersed in the gynecological cleaning liquid, the cotton sliver is placed in the vagina of an SD rat, and friction cleaning is carried out for 10min;
control group: no treatment was given.
After the washing was completed, the local vaginal tissue of SD rat was observed for congestion, edema, and abrasion, and the skin-friendly effect was evaluated.
(3) Intensity test: ultrasonic oscillation is carried out on the washing liquid based on the modified chitosan micro-nanofiber particles for 1h, and the breakage rate of the polydopamine and carboxylated modified chitosan nanofiber particles is tested.
TABLE 3 examples 1-3 and comparative examples 1-4
From Table 3, it can be seen that the chitosan fiber particles modified by the invention are not easy to break, which shows that the strength after swelling in water is better, so that the chitosan fiber particles can play a role in flexible friction for a long time when being used for cleaning, thereby remarkably improving the cleaning effect. Unmodified chitosan fiber particles are hard to swell to form gel particles, so that the particles have great damage to skin due to friction. Only carboxyl modified chitosan fiber particles are extremely easy to dissolve in water and break due to good hydrophilicity of carboxyl, and the friction cleaning effect is reduced during use. Only dopamine-modified chitosan fiber particles, because the oxidation polymerization of dopamine improves the crosslinking degree of the fibers, the fibers are difficult to absorb water and swell, and the friction injury to skin is large. In comparative example 4, when chitosan was carboxylated and modified and spun, the degree of carboxylation was substantially the same on the inner and outer surfaces of the fiber, and when the fiber was used, the solution was excessively absorbed in water and broken due to the large amount of carboxyl groups contained therein, and thus the durability in friction use was lowered.
In summary, according to the lotion based on the modified chitosan micro-nano fiber particles provided by the invention, after the chitosan gel particles are contacted with water, the liquid absorption swelling becomes soft and elastic gel particles with certain strength. When the lotion is applied to skin, chitosan gel particles in the lotion can repeatedly rub with deep pores of the skin, tiny dirt of the chitosan gel particles is peeled off from the deep pores, and microemulsion is formed through emulsification of the surfactant, so that the chitosan gel particles are removed to the surface of the skin, and the effect of thoroughly cleaning is achieved. In addition, the chitosan gel particles are soft and elastic, and can play a certain massage effect on the skin of private parts during cleaning, so that the feeling of tarnishing and pain caused by friction can be avoided.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention.
Claims (9)
1. The washing liquid based on the modified chitosan micro-nanofiber particles is characterized by comprising 0.1-3wt% of polydopamine and carboxylated modified chitosan nanofiber particles, wherein the grafting amount of carboxyl on the polydopamine and carboxylated modified chitosan nanofiber particles is sequentially reduced from outside to inside of the fiber, so that the washing liquid based on the modified chitosan micro-nanofiber particles is swelled but not dissolved during washing, and the softness and the elasticity are improved;
the preparation method of the polydopamine and carboxylation modified chitosan nanofiber particle comprises the following steps:
s1, crushing chitosan nanofiber obtained by spinning to obtain chitosan nanofiber particles with the diameter of 0.5-500 mu m and the length of 0.5-500 mu m;
s2, carrying out carboxylation grafting reaction on the chitosan nanofiber particles obtained in the step S1 in a solution with the ethanol volume content of more than 80%, so as to obtain carboxylated chitosan nanofiber particles, wherein the carboxyl grafting amount is sequentially reduced from the outside to the inside of the fiber;
s3, adding the carboxylated chitosan nanofiber particles obtained in the step S2 into a mixed solution of ethanol and water, and then adding dopamine hydrochloride to carry out a grafting reaction to obtain dopamine and carboxylated modified chitosan nanofiber particles;
s4, oxidizing and polymerizing the dopamine and carboxylated modified chitosan nanofiber particles obtained in the step S3 in a sodium periodate solution to obtain the polydopamine and carboxylated modified chitosan nanofiber particles.
2. The modified chitosan micro-nanofiber particle-based washing solution according to claim 1, wherein in the step S2, the carboxylation grafting reaction is acrylic acid grafting, and the molar ratio of acrylic acid to chitosan nanofiber particle is 1:0.1 to 20.
3. The washing liquid based on modified chitosan micro-nano fiber particles according to claim 2, wherein in the step S2, after the carboxylation grafting reaction is completed, the washing liquid is subjected to alkali washing by using a mixed solution of ethanol and water of sodium hydroxide, and then is washed to be neutral by using a mixed solution of absolute ethanol and deionized water.
4. The washing liquid based on modified chitosan micro-nano fiber particles according to claim 1, wherein in the step S3, the volume ratio of the ethanol to the water is 4:1, and the mixed solution is further added with an N-hydroxysuccinimide/1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride catalyst.
5. The washing solution based on modified chitosan micro-nanofiber particles according to claim 1, wherein in the step S3, the amino group on the dopamine hydrochloride reacts with the carboxyl group on the carboxylated chitosan nanofiber particles, and after the reaction is completed, the substitution degree of the carboxyl group is 0.2-0.3, and the substitution degree of the dopamine is 0.4-0.6.
6. The washing liquid based on modified chitosan micro-nano fiber particles according to claim 1, wherein in step S4, the time of the oxidative polymerization reaction is 10-20 hours; after the reaction is completed, the mixture is filtered, washed by ethanol and water in a volume ratio of 4:1 and dried.
7. The washing liquid based on modified chitosan micro-nano fiber particles according to claim 1, wherein the washing liquid based on modified chitosan micro-nano fiber particles comprises the following components in percentage by mass:
0.1 to 3 percent of polydopamine and carboxylated modified chitosan nanofiber particles;
5.0 to 25.0 percent of surfactant;
0.1 to 10 percent of humectant;
0.1 to 3.0 percent of thickening agent;
0.5 to 1.5 percent of conditioner;
0.1 to 0.3 percent of acidity regulator;
0.1 to 0.5 percent of preservative;
0.5 to 1.5 percent of solubilizer;
0.1 to 5.0 percent of functional active ingredient;
complexing agent 0.01-0.2%;
0.05 to 1.0 percent of essence;
92.84 to 49.0 percent of purified water.
8. The washing liquid based on modified chitosan micro-nano fiber particles according to claim 7, wherein the surfactant is one or more of cocamidopropyl betaine, sodium fatty alcohol sulfate, ammonium dodecyl sulfate, sodium lauroyl glutamate, sodium lauroyl sarcosinate, cocoyl glutamate, ammonium fatty alcohol polyoxyethylene ether sulfate, disodium cocoyl amphodiacetate, disodium laureth sulfosuccinate, cocoyl hydroxysulfobetaine, alkyl glucoside, sodium cocoyl taurate, ammonium lauroyl sulfate, cocoyl propyl betaine, sodium myristoyl sarcosinate, sodium fatty alcohol polyoxyethylene ether sulfate, cocoyl monoethanolamine, and sodium fatty acid methyl ester sulfonate;
the thickening agent is one or more of PEG-150 pentaerythritol tetrastearate, polyacrylic acid copolymer and sodium chloride;
the humectant is one or more of propylene glycol, glycerol, butanediol, sorbitol, amino acid humectant, trehalose, sodium hyaluronate, sodium polyglutamate and polyglycerol-10;
the acidity regulator is one or more of lactic acid and citric acid;
the preservative is one or more of potassium sorbate, sodium benzoate, triclosan, methylisothiazolinone, cetylpyridinium chloride, chlorpheniramine, p-hydroxyacetophenone, phenoxyethanol, benzalkonium chloride, benzalkonium bromide, bronopol, pinocele and 2, 4-dichlorobenzene alcohol;
the solubilizer is one or more of PEG-40 hydrogenated castor oil, laureth-7/laureth-9 and PEG-80 sorbitan laurate;
the functional active ingredients are one or more of ginseng extract, dipotassium glycyrrhizinate, hydrolyzed collagen, chitin, tea tree oil, menthol, borneol, aloe extract, honeysuckle extract, wild chrysanthemum extract, gingko extract, pearl hydrolysate, rose hydrosol, safflower extract, angelica extract, dandelion extract, papaya extract, tree peony root bark extract, acid bean seed extract and seaweed active peptide;
the complexing agent is one or two of disodium ethylenediamine tetraacetate and tetrasodium ethylenediamine tetraacetate.
9. The modified chitosan micro-nanofiber particle-based lotion according to claim 8, wherein the preparation method of the modified chitosan micro-nanofiber particle-based lotion comprises the following steps: adding the complexing agent into purified water, stirring until the complexing agent is completely dissolved, heating to 60-80 ℃, sequentially adding the surfactant, the humectant and the conditioner, stirring uniformly, cooling to 55-40 ℃, sequentially adding the preservative, the functional active ingredient, the polydopamine, the carboxylated modified chitosan nanofiber particles, the thickener, the solubilizer, the essence and the acidity regulator, and stirring uniformly to obtain the washing liquid based on the modified chitosan micro-nanofiber particles.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012036283A1 (en) * | 2010-09-16 | 2012-03-22 | 国立大学法人鳥取大学 | Cosmetic material, bathwater additive and pharmaceutical composition containing chitin nanofibers or chitosan nanofibers |
| CN105327339A (en) * | 2014-08-15 | 2016-02-17 | 人福医药集团医疗用品有限公司 | Chitosan gel particle lotion and preparation method thereof |
| CN109180970A (en) * | 2018-08-30 | 2019-01-11 | 武汉理工大学 | A kind of citric acid cross-linked chitosan and the hydrogel of dopamine and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012036283A1 (en) * | 2010-09-16 | 2012-03-22 | 国立大学法人鳥取大学 | Cosmetic material, bathwater additive and pharmaceutical composition containing chitin nanofibers or chitosan nanofibers |
| CN105327339A (en) * | 2014-08-15 | 2016-02-17 | 人福医药集团医疗用品有限公司 | Chitosan gel particle lotion and preparation method thereof |
| CN109180970A (en) * | 2018-08-30 | 2019-01-11 | 武汉理工大学 | A kind of citric acid cross-linked chitosan and the hydrogel of dopamine and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 多巴胺氧化自聚合反应及其改性海藻酸钠水凝胶的制备与载药性能研究;高博;中国优秀硕士学位论文全文数据库 工程科技I辑(第03期);摘要，3.4实验结果讨论，3.5本章小结，4.1主要研究结论 * |
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