CN114272159A - 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 solution based on modified chitosan micro-nano fiber particles, which comprises 0.1-3 wt% of polydopamine and carboxylation modified chitosan nano fiber particles, a complexing agent, a thickening agent, a humectant, functional active ingredients and the like. Wherein, the grafting amount of carboxyl on the polydopamine and carboxylation modified chitosan nano fiber particles is reduced from the outside to the inside of the fiber in sequence, so that the washing liquid is swelled and not dissolved when being washed, and the softness and the elasticity are improved. The carboxyl on the surfaces of the polydopamine and carboxylation modified chitosan nano fiber particles has high hydrophilicity, and can endow the micro-nano fiber particles with the capability of swelling to form gel particles, and the polydopamine on the surfaces can improve the gel strength of the gel particles formed after imbibition, so that the dissolution is avoided; the fiber particle surface also has positively charged amino groups, which can endow the micro-nano fiber particles with good antibacterial performance. The washing liquid provided by the invention has obvious friction washing effect and washing experience and 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 cleaning solution based on modified chitosan micro-nano fiber particles.
Background
Gynecological diseases such as vaginitis, cervicitis, cervical erosion, etc. are easy to show symptoms such as itching, abnormal leucorrhea, burning of lower body, etc. The occurrence of gynecological inflammation is closely related to the constitution and the living habits of the woman, the causes of the gynecological inflammation are complex and various, the gynecological inflammation brings a great deal of implicit information to the woman, and the living quality and the family harmony of the woman are seriously influenced. At present, more lotion for treating gynecological diseases mainly comprises two categories of traditional Chinese medicine lotion and western medicine lotion, but the two lotions have respective defects, for example, the traditional Chinese medicine lotion has weak potency and long treatment time, while the western medicine lotion has few medicinal components, single action and easy irritation, and the traditional Chinese medicine lotion and the western medicine lotion are easy to cause relapse after stopping administration and have the defects of long treatment course.
Most of the existing lotion in the current market does not contain an abrasive, and can not thoroughly clean the intractable dirt hidden in private parts; in addition, most of the private lotion also contains powerful bactericidal components, for example, Chinese patent publication No. CN103263525A, publication No. 2013, 08 and 28 days, with the title of "gynecological lotion and preparation method thereof", discloses a lotion formula containing high-concentration Chinese herbal medicine extract, Chinese patent publication No. CN103446177A, publication No. 2013, 12 and 18 days, with the title of "lotion for treating gynecological diseases and preparation method thereof", and discloses a lotion formula containing chlorhexidine. The medicines such as the high-efficiency bactericidal components and the like are easy to cause the human body to generate dependence on the medicines after long-term use, destroy the balance of the natural flora in the private parts, interfere the self-cleaning capability of the private parts, generate certain irritation to the tender skin of the private parts and have certain side effects.
Patent CN1823813A discloses a female vaginal nursing therapeutic composition, which utilizes the antibacterial property and biocompatibility of chitosan or its cationic derivative to solve the problem of drug resistance. However, the cleaning effect is still not ideal because the cleaning solution used in the patent is still soluble. However, when the cleaning liquid is used for cleaning a human body, the addition of the abrasive to the cleaning liquid for nursing the human body is rarely seen in the prior art because the abrasive is needed to be considered to be harmful to the human body.
In view of the above, there is a need to design an improved lotion based on modified chitosan micro-nanofiber particles to solve the above problems.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the washing liquid based on the modified chitosan micro-nano fiber particles, and the softness, elasticity and wear resistance of the fiber particles in the washing liquid are improved by modifying the chitosan fiber particles with carboxyl and dopamine, so that the friction washing effect is improved, and the friction pain is reduced.
In order to achieve the above object, the present invention provides a washing solution based on modified chitosan micro-nano fiber particles, comprising 0.1 wt% to 3 wt% of polydopamine and carboxylated modified chitosan nano fiber particles, wherein the graft amount of carboxyl groups on the polydopamine and carboxylated modified chitosan nano fiber particles is reduced from the outside to the inside of the fiber, so that the washing solution based on modified chitosan micro-nano fiber particles is swollen but not dissolved during washing, and the softness and elasticity are improved.
As a further improvement of the invention, the preparation method of the polydopamine and carboxylation modified chitosan nanofiber particle comprises the following steps:
s1, crushing chitosan nano-fiber obtained by spinning to obtain chitosan nano-fiber particles with the diameter of 0.5-500 mu m and the length of 0.5-500 mu m;
s2, performing carboxylation grafting reaction on the chitosan nano-fiber particles obtained in the step S1 in a solution with the ethanol volume content of more than 80% to obtain carboxylated chitosan nano-fiber 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 perform a grafting reaction to obtain dopamine and carboxylated modified chitosan nanofiber particles;
s4, carrying out oxidative polymerization on 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 carboxylated grafting reaction uses acrylic acid grafting, and the molar ratio of the acrylic acid to the chitosan nanofiber particles is 1: 0.1 to 20.
As a further improvement of the present invention, in step S2, after the carboxylation grafting reaction is completed, a mixed solution of ethanol and water of sodium hydroxide is used for alkali washing, and then a mixed solution of anhydrous ethanol and deionized water is used for washing until the mixture is neutral.
As a further improvement of the present invention, in step S3, the volume ratio of ethanol to water is 4:1, and an NHS/EDC (N-hydroxysuccinimide/(1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride)) catalyst is further added to the mixed solution.
As a further improvement of the 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 degree of substitution of the carboxyl group is 0.2-0.3, and the degree of substitution of dopamine is 0.4-0.6.
As a further improvement of the invention, in the step S4, the time of the oxidative polymerization reaction is 10-20 h; after the reaction is finished, filtering, washing with ethanol and water in a volume ratio of 4:1, and drying.
As a further improvement of the invention, the washing liquor based on the modified chitosan micro-nanofiber particles comprises the following components in percentage by mass:
0.1 to 3 percent of polydopamine and carboxylation modified chitosan nano-fiber 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 ingredients;
0.01 to 0.2 percent of complexing agent;
0.05 to 1.0 percent of essence;
92.84 to 49.0 percent of purified water.
As a further improvement of the present invention, the surfactant is one or more of cocamidopropyl betaine, sodium fatty alcohol sulfate, ammonium lauryl sulfate, sodium lauroyl glutamate, sodium lauroyl sarcosinate, cocoyl glutamic acid, ammonium fatty alcohol polyoxyethylene ether sulfate, disodium cocoyl amphodiacetate, disodium laureth sulfosuccinate, cocoyl hydroxysultaine, alkyl glucoside, sodium cocoyl taurate, ammonium lauryl sulfate, 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 antiseptic is one or more of potassium sorbate, sodium benzoate, triclosan, MIT (methylisothiazolinone), cetylpyridinium chloride, chlorphenesin, p-hydroxyacetophenone, phenoxyethanol, benzalkonium chloride, benzalkonium bromide, bronopol, kaempferol and 2, 4-dichlorobenzyl alcohol;
the solubilizer is one or more of PEG-40 hydrogenated castor oil, laureth-7/laureth-9 and PEG-80 sorbitan lauric acid;
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, ginkgo extract, pearl hydrolysate, rose hydrosol, safflower extract, angelica extract, dandelion extract, papaya extract, peony root bark extract, tamarind seed extract and seaweed active peptide;
the stability is one or two of disodium ethylene diamine tetraacetate (disodium EDTA) and tetrasodium ethylene diamine tetraacetate (tetrasodium EDTA).
As a further improvement of the invention, the preparation method of the washing liquor 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 a surfactant, a humectant and a conditioner, uniformly stirring, cooling to 55-40 ℃, sequentially adding a preservative, a functional active ingredient, polydopamine, a carboxylated modified chitosan nano-fiber particle, a thickening agent, a solubilizer, essence and an acidity regulator, and uniformly stirring to obtain the washing liquor based on the modified chitosan micro-nano-fiber particle.
The invention has the beneficial effects that:
the washing liquor based on the modified chitosan micro-nano fiber particles provided by the invention has the advantages that the adopted chitosan nano fiber particles have high specific surface area and high biocompatibility, the fiber surface roughness is relatively high, and the friction cleaning effect is good. After the poly-dopamine and the carboxyl are simultaneously modified, on one hand, the affinity of the carboxyl and the catechol group of the dopamine to dirt is improved, and certain substances 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 but not dissolved in water, the wear resistance is good, and the chitosan fiber particles can be repeatedly rubbed and used without cracking; the softness and elasticity of the swelled fiber particles become excellent, the friction comfort is improved, and the harm to human bodies is reduced. The chitosan gel particles in the lotion can repeatedly rub against the deep layer of skin pores to strip off tiny dirt from the deep layer of the pores, and the microemulsion is formed through the emulsification of the surfactant and removed to the surface of the skin, so that the effect of thorough 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 invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in detail below with reference to specific embodiments.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the scheme of the present invention are shown in the specific embodiments, and other details not closely related to the present invention are omitted.
In addition, it is also to be 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 solution based on the modified chitosan micro-nano fiber particles comprises 0.1-3 wt% of polydopamine and carboxylation modified chitosan nano fiber particles, and the grafting amount of carboxyl groups on the polydopamine and carboxylation modified chitosan nano fiber particles is reduced from the outside to the inside of the fiber in sequence, so that the washing solution based on the modified chitosan micro-nano fiber particles is swelled and insoluble during washing, and the softness and the elasticity are improved. By the operation, the adopted chitosan nano fiber particles have high specific surface area and high biocompatibility, the surface roughness of the fiber is relatively high, and the friction cleaning effect is good. After the poly-dopamine and the carboxyl are simultaneously modified, on one hand, the affinity of the carboxyl and the catechol group of the dopamine to dirt is improved, and certain substances 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 but not dissolved in water, the wear resistance is good, and the chitosan fiber particles can be repeatedly rubbed and used without cracking; the softness and elasticity of the swelled fiber particles become excellent, the friction comfort 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 nano-fiber particles comprises the following steps:
s1, crushing chitosan nano-fiber obtained by spinning to obtain chitosan nano-fiber particles with the diameter of 0.5-500 mu m and the length of 0.5-500 mu m; the degree of deacetylation of the chitosan starting material was about 1.
S2, performing carboxylation grafting reaction on the chitosan nano-fiber particles obtained in the step S1 in a solution (preferably all ethanol) with the ethanol volume content of more than 80% to obtain carboxylated chitosan nano-fiber particles, wherein the carboxyl grafting amount is sequentially reduced from the outside to the inside of the fiber; the carboxylation grafting reaction is preferably grafted by acrylic acid, and the molar ratio of the acrylic acid to the chitosan nanofiber particles is 1: 0.1-20, preferably 0.8-3, more preferably 1-2; the substitution degree of carboxyl is 0.7-0.8, calculated according to the content of substituted amino in the original amino. In the step, because the chitosan nano fiber particles are insoluble in ethanol, the extension degree of chitosan molecular chains is limited, so that acrylic acid is mainly grafted on the surface layer, and the graft substitution degree in the fiber is ensured to be less than 0.2 by controlling the reaction time. In this way, the solubility of the nanofiber particles during washing can be reduced, and the loss of the friction washing effect due to dissolution can be prevented. The internal substitution degree is small, the skeleton structure of the nanofiber particles can be kept, and then 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 perform a grafting reaction to obtain dopamine and carboxylated modified chitosan nanofiber particles; referring to fig. 1, the amino group and the carboxyl group of the dopamine hydrochloride undergo amidation grafting reaction, so that a part of the carboxyl group is further substituted by the dopamine hydrochloride, and after the reaction is completed, the degree of substitution of the carboxyl group is 0.2 to 0.3, and the degree of substitution of the dopamine is 0.4 to 0.6.
S4, carrying out oxidative polymerization on 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, the strength of the chitosan fiber particles is further improved, and when the chitosan gel particles contact water, the chitosan gel particles absorb the liquid and swell to become soft and elastic gel particles with certain strength. When the lotion is applied to the skin, the chitosan gel particles in the lotion can repeatedly rub against the deep layer of skin pores to strip off tiny dirt from the deep layer of the pores, and the microemulsion is formed through the emulsification of the surfactant and is removed to the surface of the skin, so that the effect of thorough cleaning is achieved. In addition, the chitosan gel particles are soft and elastic, can play a certain massage effect on the private skin when being cleaned, and can not bring the feeling of tarnish and pain due to friction.
Examples 1 to 3
The washing lotion based on the modified chitosan micro-nano fiber particles provided by the embodiments 1 to 3 has the component contents shown in table 1.
The preparation method comprises the following steps: adding a complexing agent into purified water according to the mass percentage, stirring until the complexing agent is completely dissolved, heating to 60-80 ℃, sequentially adding a surfactant, a humectant and a conditioner, uniformly stirring, cooling to 55-40 ℃, sequentially adding a preservative, a functional active ingredient, polydopamine, a carboxylated modified chitosan nano-fiber particle, a thickening agent, a solubilizer, essence and an acidity regulator, and uniformly stirring to obtain the washing liquor based on the modified chitosan micro-nano fiber particle.
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 particle is 20 microns, the length of the chitosan micro-nano fiber particle is 80 microns, and the chitosan micro-nano fiber particle is prepared by crushing chitosan nano fiber 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 1 g: 30mL, adding acrylic acid into a mixed solution of the chitosan micro-nanofiber particles and ethanol, wherein the molar ratio of the acrylic acid to the amino groups of the chitosan micro-nanofiber particles is 1: 1.5, stirring uniformly at room temperature, and heating to 40-60 ℃ for reaction in a constant-temperature water bath for 4-48 hours. After the reaction is finished, filtering, and performing alkali washing on the carboxylated chitosan micro-nano fiber particles to strong alkalinity by using alkali liquor prepared by sodium hydroxide (the alkali liquor is obtained by dissolving 32g of sodium hydroxide in 800ml of deionized water and then adding 3400ml of absolute ethyl alcohol, namely the alkali liquor consists of 4% of sodium hydroxide and absolute ethyl alcohol in a volume ratio of 4: 17); 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 then 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-nano fiber particles with a carboxyl substitution degree of 0.7-0.8 in ethanol/water (volume ratio of 4:1), reacting at room temperature for 24 hours 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 chitosan micro-nano fiber particles grafted with dopamine groups and carboxyl groups, 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 (the solid-to-liquid ratio is 1: 50), adding 5% of sodium periodate solution, and reacting for 12 hours at room temperature. And after the reaction is finished, filtering, washing with ethanol/water (volume ratio is 4:1), and drying to obtain carboxyl chitosan @ polydopamine (CECS @ Poly Dopa) micro-nano fiber particles.
TABLE 1 component ratios for examples 1-3
Comparative example 1
Compared with example 1, the difference is that polydopamine and carboxylated modified chitosan nanofiber particles are replaced with unmodified chitosan nanofiber particles. The rest is substantially the same as that of embodiment 1, and will not be described herein.
Comparative example 2
Compared with example 1, the difference is that polydopamine and carboxylation modified chitosan nanofiber particles are replaced by carboxylation modified chitosan nanofiber particles, namely steps (3) and (4) in example 1 are removed. The rest is substantially the same as that of embodiment 1, and will not be described herein.
Comparative example 3
Compared with example 1, the difference is that polydopamine and carboxylated modified chitosan nanofiber particles are replaced by dopamine modified chitosan nanofiber particles, namely step (2) in example 1 is removed, and polydopamine is adhered to the surface of chitosan fibers in a physical coating form. The rest is substantially the same as that of embodiment 1, and will not be described herein.
Comparative example 4
Compared with the example 1, the difference is that chitosan is carboxylated and then spun, and then dopamine modification in the steps (3) and (4) is carried out, and the degree of carboxylation on the inner surface and the outer surface of the fiber is basically the same. The rest is substantially the same as that of embodiment 1, and will not be described herein.
The lotions of examples 1 to 3 and comparative examples 1 to 4 were subjected to vaginal washing efficacy test, skin-friendly test and abrasion resistance test.
(1) And (3) vagina cleaning curative effect testing: the gynecological cleaning fluid is directly filled into a vaginal irrigator, then the vaginal irrigator is inserted into a vaginal extrusion bottle body for irrigation, the irrigation is carried out for 2 times every day, each time lasts for 2-3 min, 5 consecutive days are taken as a treatment course, and the curative effect is evaluated after the treatment course is used.
Judgment of therapeutic effect
And (3) healing: the subjective symptoms disappear, the vagina is clean (I), the vagina swab is cultured to turn negative, and the negative result is obtained after 4 times of menstruation;
the method has the following advantages: the subjective symptom is relieved, the vagina is clean (II), only a few bacteria grow in the vagina swab culture, at most 10 trichomonas or mould are occasionally seen, and the positive person is rechecked for 2 times after 4 times of menstruation; the total cure and effective rate is the total effective rate.
And (4) invalidation: no improvement of subjective symptoms, no change of vaginal cleanliness and no change of 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 washing solutions of comparative examples 1 to 4, respectively.
TABLE 2 cleaning efficacy test results
As can be seen from Table 2, the chitosan fiber particles modified by the present invention have good cleaning effect on both mycotic vaginitis and bacterial vaginitis. And the swelling and crushing rate test of the chitosan fiber particle is combined, so that the chitosan fiber particle basically has no harm to skin, has good cleaning experience, and can realize deep cleaning. And the cleaning effect is obviously reduced by adopting the unmodified chitosan fiber particles, because the unmodified chitosan fiber particles cannot swell to form gel and the flexible friction effect is poor. The chitosan fiber particle modified with only carboxyl group was improved compared to the unmodified one, but was still lower than that of example 1, because the strength was lower, and the chitosan fiber particle was easily broken during washing, resulting in a decrease in the friction washing effect. The cleaning effect of the chitosan fiber particles modified by dopamine only is higher than that of unmodified chitosan fiber particles and lower than that of carboxyl modified chitosan fiber particles, and the test results in table 3 show that the chitosan fiber particles modified by dopamine only have improved strength due to crosslinking, but are still difficult to absorb water and swell to form gel, so the friction cleaning effect is poor.
(2) Skin-friendly testing: test groups and control groups were established, and 10 adult healthy SD rats were each group.
Test groups: after the gynecological cleaning fluid is soaked in the cotton sliver, the cotton sliver is placed in the vagina of an SD rat and is rubbed and cleaned for 10 min;
control group: without any treatment.
After the completion of the washing, the phenomena of congestion, edema and abrasion of local vaginal tissues of SD rats were observed, and the skin-friendly effect was evaluated.
(3) And (3) testing the strength: the washing liquid based on the modified chitosan micro-nano fiber particles prepared by the invention is subjected to ultrasonic oscillation for 1h, and the breaking rate of polydopamine and carboxylation modified chitosan nano fiber particles is tested.
TABLE 3 of examples 1 to 3 and comparative examples 1 to 4
As can be seen from Table 3, 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 of flexible friction for a long time when being used for cleaning, thereby obviously improving the cleaning effect. Unmodified chitosan fiber particles are difficult to swell to form gel particles, and therefore are more abrasive to the skin. The chitosan fiber particles modified only by carboxyl are easy to dissolve in water and break due to good hydrophilicity of the carboxyl, and the friction cleaning effect is reduced when the chitosan fiber particles are used. The chitosan fiber particles modified by dopamine are difficult to absorb water and swell due to the fact that the crosslinking degree of the fibers is improved by oxidative polymerization of dopamine, and the damage to skin caused by friction is large. In comparative example 4, when chitosan was first carboxylated and then spun, the degree of carboxylation on the inner and outer surfaces of the fiber was substantially the same, and in use, the solution was broken due to excessive water absorption because of the presence of a large amount of carboxyl groups in the inside, and thus the durability in use by friction was lowered.
In conclusion, when the chitosan gel particles contact water, the lotion based on the modified chitosan micro-nanofiber particles provided by the invention absorbs the water and swells to form the soft and elastic gel particles with certain strength. When the lotion is applied to the skin, the chitosan gel particles in the lotion can repeatedly rub against the deep layer of skin pores to strip off tiny dirt from the deep layer of the pores, and the microemulsion is formed through the emulsification of the surfactant and is removed to the surface of the skin, so that the effect of thorough cleaning is achieved. In addition, the chitosan gel particles are soft and elastic, can play a certain massage effect on the private skin when being cleaned, and can not bring the feeling of tarnish and pain due to friction.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the present invention.
Claims (10)
1. The washing liquor based on the modified chitosan micro-nano fiber particles is characterized by comprising 0.1-3 wt% of polydopamine and carboxylation modified chitosan nano fiber particles, wherein the grafting amount of carboxyl groups on the polydopamine and carboxylation modified chitosan nano fiber particles is reduced from the outside to the inside of the fiber, so that the washing liquor based on the modified chitosan micro-nano fiber particles is swelled and not dissolved when being washed, and the softness and the elasticity are improved.
2. The washing lotion based on the modified chitosan micro-nano fiber particles as claimed in claim 1, wherein the preparation method of the polydopamine and carboxylated modified chitosan nano fiber particles comprises the following steps:
s1, crushing chitosan nano-fiber obtained by spinning to obtain chitosan nano-fiber particles with the diameter of 0.5-500 mu m and the length of 0.5-500 mu m;
s2, performing carboxylation grafting reaction on the chitosan nano-fiber particles obtained in the step S1 in a solution with the ethanol volume content of more than 80% to obtain carboxylated chitosan nano-fiber 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 perform a grafting reaction to obtain dopamine and carboxylated modified chitosan nanofiber particles;
s4, carrying out oxidative polymerization on 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.
3. The washing lotion based on modified chitosan micro-nano fiber particles of claim 2, wherein in step S2, the carboxylated grafting reaction is performed by acrylic acid grafting, and the molar ratio of acrylic acid to chitosan nano fiber particles is 1: 0.1 to 20.
4. The washing liquid based on the modified chitosan micro-nano fiber particles of claim 3, wherein in step S2, after the carboxylation grafting reaction is completed, the washing liquid is alkaline washed by a mixed solution of ethanol and water of sodium hydroxide, and then washed to be neutral by a mixed solution of anhydrous ethanol and deionized water.
5. The washing lotion based on the modified chitosan micro-nano fiber particles as claimed in claim 2, wherein in step S3, the volume ratio of ethanol to water is 4:1, and an N-hydroxysuccinimide/(1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride) catalyst is further added to the mixed solution.
6. The washing lotion based on the modified chitosan micro-nano fiber particles of claim 2, wherein in step S3, the amino group on the dopamine hydrochloride reacts with the carboxyl group on the carboxylated chitosan nano fiber particles, and after the reaction is completed, the degree of substitution of the carboxyl group is 0.2-0.3, and the degree of substitution of dopamine is 0.4-0.6.
7. The washing lotion based on the modified chitosan micro-nano fiber particles of claim 2, wherein in the step S4, the time of the oxidative polymerization reaction is 10-20 h; after the reaction is finished, filtering, washing with ethanol and water in a volume ratio of 4:1, and drying.
8. The washing liquid based on the modified chitosan micro-nano fiber particles as claimed in claim 1, wherein 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 carboxylation modified chitosan nano-fiber 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 ingredients;
0.01 to 0.2 percent of complexing agent;
0.05 to 1.0 percent of essence;
92.84 to 49.0 percent of purified water.
9. The washing lotion based on modified chitosan micro-nano fiber particles of claim 8, wherein the surfactant is one or more of cocamidopropyl betaine, sodium fatty alcohol sulfate, ammonium lauryl sulfate, sodium lauroyl glutamate, sodium lauroyl sarcosinate, cocoyl glutamic acid, ammonium fatty alcohol polyoxyethylene ether sulfate, disodium cocoyl amphodiacetate, disodium laureth sulfosuccinate, cocoyl hydroxysultaine, alkyl glucoside, sodium cocoyl taurate, ammonium lauryl 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, chlorphenesin, p-hydroxyacetophenone, phenoxyethanol, benzalkonium chloride, benzalkonium bromide, bronopol, kaempferol and 2, 4-dichlorobenzyl alcohol;
the solubilizer is one or more of PEG-40 hydrogenated castor oil, laureth-7/laureth-9 and PEG-80 sorbitan lauric acid;
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, ginkgo extract, pearl hydrolysate, rose hydrosol, safflower extract, angelica extract, dandelion extract, papaya extract, peony root bark extract, tamarind seed extract and seaweed active peptide;
the stability is one or two of disodium ethylene diamine tetraacetate and tetrasodium ethylene diamine tetraacetate.
10. The washing lotion based on the modified chitosan micro-nano fiber particles as claimed in claim 9, wherein the preparation method of the washing lotion based on the modified chitosan micro-nano fiber particles comprises: adding the complexing agent into purified water, stirring until the complexing agent is completely dissolved, heating to 60-80 ℃, sequentially adding a surfactant, a humectant and a conditioner, uniformly stirring, cooling to 55-40 ℃, sequentially adding a preservative, a functional active ingredient, polydopamine, a carboxylated modified chitosan nano-fiber particle, a thickening agent, a solubilizer, essence and an acidity regulator, and uniformly stirring to obtain the washing liquor based on the modified chitosan micro-nano-fiber particle.
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| 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 |
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| 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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| 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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