CN115300415A

CN115300415A - Preparation method of carboxymethyl cellulose fiber mask

Info

Publication number: CN115300415A
Application number: CN202211125218.0A
Authority: CN
Inventors: 俞月渊; 俞周杰
Original assignee: Shenzhen Qianhaigangying Biotechnology Co ltd
Current assignee: Shenzhen Qianhaigangying Biotechnology Co ltd
Priority date: 2022-09-15
Filing date: 2022-09-15
Publication date: 2022-11-08
Anticipated expiration: 2042-09-15
Also published as: CN115300415B

Abstract

The invention relates to the field of fiber masks, and particularly discloses a preparation method of a carboxymethyl cellulose fiber mask, which comprises the following steps: step 1, preparing a mask base cloth: (1) dispersing fibers; (2) preparing triacetyl gallic acid; (3) modified carboxymethyl cellulose fiber; (4) modified carboxymethyl cellulose fiber mask base cloth; step 2, preparing facial mask liquid: mixing the plant extract, the humectant, the thickening agent, the emulsifier, the preservative, the pH regulator and deionized water, and uniformly stirring to form a mixed solution, namely facial mask solution; step 3, preparing the facial mask: and completely soaking the mask base cloth in the mask liquid to finish the preparation of the mask. Aiming at the improvement of the existing mask, the invention mainly focuses on the improvement of the mask base cloth, so that the mask base cloth also has the advantages of high strength, good toughness and good antibacterial activity on the basis of high water absorption and high water retention, thus no preservative is required to be added in the mask liquid, and the harm of the preservative to the health of human bodies is reduced.

Description

Preparation method of carboxymethyl cellulose fiber mask

Technical Field

The invention relates to the field of fiber masks, and particularly relates to a preparation method of a carboxymethyl cellulose fiber mask.

Background

Carboxymethylcellulose (CMC), a carboxymethylated derivative of cellulose, also known as cellulose gum, is the most ionic cellulose gum. CMC is generally an anionic high molecular compound obtained by reacting natural cellulose with caustic alkali and monochloroacetic acid, and the molecular weight of the compound varies from several thousand to millions. CMC belongs to the modification of natural cellulose, and is formally called as modified cellulose by grain agriculture organization (FAO) and World Health Organization (WHO) of the United nations at present. The synthesis method of sodium carboxymethylcellulose is invented by German E.Jansen in 1918, and is patented in 1921 and is commercially produced in Europe since then. CMC was only a crude product at that time and was used as a colloid and binder. In 1936-1941, the industrial use of sodium carboxymethylcellulose was quite actively studied, several quite inspiring patents were published, and during world war ii, CMC was used in synthetic detergents in germany as an anti-redeposition agent and as a substitute for certain natural gums (e.g. gelatin, gum arabic), leading to a great development of the CMC industry. Therefore, the research and development of the novel cellulose material are paid attention by researchers at home and abroad, and the yield and the water content of the biological cellulose composite membrane are improved by adding the carboxymethyl cellulose so that the produced composite membrane can better meet the requirement of serving as a mask material.

Chinese patent document CN201811489908.8 discloses an alginate fiber mask base cloth and a preparation method thereof. The base cloth of the mask consists of carboxymethyl cellulose fibers, calcium alginate fibers and sodium alginate. The composite fabric is prepared by mixing and processing carboxymethyl cellulose fibers and calcium alginate fibers into mixed fibers and then soaking the mixed fibers in a sodium alginate aqueous solution, and the water absorption capacity and the water retention capacity of the mask base fabric are improved. However, the calcium alginate fibers are brittle and hard and have low strength, so that the flexibility of the base cloth of the carboxymethyl cellulose fiber facial mask is influenced by blending the calcium alginate fibers and the carboxymethyl cellulose fiber facial mask, and in addition, the bacteriostatic performance of the fiber facial mask is insufficient. Therefore, the mask cloth composed of the carboxymethyl cellulose fiber is prepared, and has the characteristics of high water absorption and retention performance, high strength, good toughness and antibacterial activity.

Disclosure of Invention

Aiming at the problems in the prior art, the invention aims to provide a preparation method of a carboxymethyl cellulose fiber facial mask.

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

the invention provides a preparation method of a carboxymethyl cellulose fiber facial mask, which comprises the following steps:

step 1, preparing a mask base cloth:

(1) Dispersing fibers:

mixing carboxymethyl cellulose fiber and chitosan fiber in deionized water, dropwise adding an acetic acid solution, then placing in a constant-temperature water bath kettle for heating reaction, then cooling to room temperature, purifying and drying, and placing the obtained mixed fiber in N, N-dimethylformamide to form a uniform solution to obtain a fiber dispersion liquid;

(2) Preparing triacetyl gallic acid:

mixing p-toluenesulfonic acid and acetic anhydride, stirring uniformly, adding dried gallic acid, placing in a constant temperature water bath kettle, heating, stirring, reacting, naturally cooling to room temperature, adding into deionized water, mixing uniformly, dropwise adding hydrochloric acid until the pH is 1.0-1.5, and generating a large amount of precipitate, and then extracting and drying to obtain triacetyl gallic acid;

(3) Modified carboxymethyl cellulose fiber:

sequentially adding alpha-cyclodextrin, geraniol and triacetyl gallic acid into the fiber dispersion liquid, stirring uniformly, adding a catalyst, heating, stirring for reaction, naturally cooling to room temperature, adding the cooled catalyst into glacial ethyl ether for precipitation, quickly filtering out the precipitate, recrystallizing, and drying under reduced pressure to obtain modified carboxymethyl cellulose fibers;

(4) Modified carboxymethyl cellulose fiber mask base cloth:

dissolving the modified carboxymethyl cellulose fiber in N, N-dimethylformamide to form a uniform solution, taking the uniform solution as a spinning solution, and obtaining the mask base cloth through an electrostatic spinning technology;

step 2, preparing facial mask liquid:

mixing the plant extract, the humectant, the thickening agent, the emulsifier, the preservative, the pH regulator and deionized water, and uniformly stirring to form a mixed solution, namely facial mask solution;

step 3, preparing the facial mask:

and completely soaking the mask base cloth in the mask liquid, starting ultrasound, taking out the mask base cloth after the ultrasound is finished, and folding and packaging the mask base cloth soaked with the mask liquid to finish the preparation of the mask.

Preferably, in the step 1 (1), the mass fraction of the acetic acid solution is 15% to 20%, and the addition amount of the acetic acid solution is based on the mass content of acetic acid in the final solution being 1%.

Preferably, in the step 1 (1), the temperature in the thermostatic waterbath is 45-55 ℃, and the stirring time is 1-2h.

Preferably, in the step 1 (1), the density of the carboxymethyl cellulose fiber is 1.2g/cm ³ The deacetylation degree of the chitosan fiber is 90-95%; the solid-liquid ratio (the ratio of solid mass to liquid volume) of the carboxymethyl cellulose fiber, the chitosan fiber and the deionized water is 1-3.

Preferably, in the step 1 (1), the purification is performed by using a dialysis bag purification method, and the molecular weight cut-off is 10000Da; the drying is vacuum drying at 50 deg.C for 12h.

Preferably, in the step 1 (1), the solid-to-liquid ratio of the mixed fiber to the N, N-dimethylformamide is 1:6-10.

Preferably, in the step 1 (2), the weight ratio of gallic acid, p-toluenesulfonic acid and acetic anhydride is 12-17.

Preferably, in the step 1 (2), the temperature of the constant-temperature water bath is 60-70 ℃, and the stirring reaction is carried out for 2-3h.

Preferably, in the step 1 (2), deionized water is added in an amount of 2 times the volume of the reaction solution.

Preferably, in the step 1 (2), ethyl acetate is used for extraction, and the extraction times are three times; the drying is vacuum drying.

Preferably, in the step 1 (3), the mass ratio of the α -cyclodextrin, the geraniol, the triacetyl gallic acid to the fiber dispersion is 1.2 to 1.6.

Preferably, in the step 1 (3), the catalyst is p-toluenesulfonic acid, and the addition amount of the p-toluenesulfonic acid is 0.2-0.8% of the mass of the fiber dispersion.

Preferably, in the step 1 (3), the temperature is increased to 130-160 ℃, and the stirring reaction is carried out for 4-6h.

Preferably, in step 1 (3), the volume of the glacial ethyl ether is 2 times of the volume of the reaction solution, and the recrystallization is carried out by using a water/ethanol system.

Preferably, in step 1 (4), the electrospinning device is configured to: the temperature is room temperature, the spinning voltage is 20-50kv, the distance between the needle head and the receiving plate is 20cm, the spinning speed is 1-2mL/h, and the receiving plate receives the film-forming material and then dries in a drying oven.

Preferably, in the step 2, the weight ratio of the plant extract, the humectant, the thickener, the emulsifier, the pH regulator and the deionized water is 3-6.

Preferably, in the step 2, the plant extract includes at least one of peony root extract, gallnut extract, rheum palmatum extract, scutellaria baicalensis root extract, cnidium fruit extract, glycyrrhiza glabra extract, sea buckthorn oil extract, geranium extract, alfalfa extract, white peony root extract, lily extract and arbutin extract.

Preferably, in the step 2, the humectant comprises at least one of glycerin, mannitol, glycine, 1,3-propylene glycol, 1-3 butanediol, polyethylene glycol, PEG/PPG-17/6 copolymer and sodium hyaluronate.

Preferably, in step 2, the thickener comprises xanthan gum and/or carbomer.

Preferably, in the step 2, the emulsifier comprises at least one of sorbitan fatty acid ester, PPG-26-butanol polyether-26 and PEG-40 hydrogenated castor oil.

Preferably, in the step 2, the preservative comprises at least one of glyceryl caprylate, p-hydroxyacetophenone and caprylhydroxamic acid.

Preferably, in the step 2, the pH regulator includes citric acid and/or sodium citrate.

Preferably, in the step 3, the process of completely soaking the mask base cloth in the mask solution is as follows: placing the prepared facial mask liquid in a wide-mouth and clean container, slowly placing the prepared facial mask base cloth on the surface of the facial mask liquid after the prepared facial mask base cloth is unfolded, and slowly pressing the prepared facial mask liquid into the facial mask liquid after the surface of the facial mask liquid is completely unfolded.

Preferably, in the step 3, the ultrasonic treatment is carried out in an ultrasonic instrument, the ultrasonic temperature is 25-45 ℃, the ultrasonic power is 300-800W, and the ultrasonic time is 0.5-3h.

Preferably, in the step 3, the mask base cloth is taken out to be above the mask liquid, and folding and packaging are carried out until the dripping speed of the mask liquid is lower than 2 seconds per drop.

The beneficial effects of the invention are as follows:

1. in the invention, the mask base cloth and the mask liquid are respectively prepared, and the mask is obtained by combining the mask base cloth and the mask liquid. The facial mask base cloth is prepared by using carboxymethyl cellulose fibers as a main body, forming mixed fibers by using chitosan fibers as an auxiliary body, then performing modification treatment to obtain modified carboxymethyl cellulose fibers, and finally performing electrostatic spinning. The invention aims at the improvement of the existing mask and mainly focuses on the improvement of the mask base cloth, so that the mask base cloth has the advantages of high strength, good toughness and good antibacterial activity on the basis of high water absorption and high water retention, and the preservative is not required to be added in the mask liquid, thereby reducing the harm of the preservative to the health of human bodies.

2. The facial mask liquid prepared by the invention is added with various plant extractant components, which have the effects of resisting oxidation, fading color spots and repairing facial cutin, and part of the facial mask liquid has certain fragrance and corrosion resistance, so that the matching and using effects of the facial mask liquid and the mask surface base cloth are better, and the faint scent taste and the corrosion resistance effect in a short time can be kept without additionally adding essence and corrosion resistance components.

3. In the preparation process of the mask base cloth, the carboxymethyl cellulose fiber and the chitosan fiber are subjected to acidification treatment, so that the carboxymethyl cellulose fiber is acidified, the activity is enhanced, and the carboxymethyl cellulose fiber and the chitosan fiber can be mutually crosslinked.

4. In the process of preparing triacetyl gallic acid, the gallic acid is acylated, so that the steric effect of phenolic hydroxyl in the gallic acid is eliminated, and the activity of carboxyl is improved.

5. The cyclodextrin as solubilizer can increase the solubility of the hydrophobic steroid, and the special cavity structure can encapsulate the natural compound substrate, thereby improving the bioavailability and yield of the natural compound. In the invention, the cyclodextrin not only shows the inclusion property, but also utilizes a large amount of hydroxyl contained in cyclodextrin molecules to be esterified and combined with triacetyl gallic acid as a reactant.

6. The chitosan fiber structure chain has abundant free-OH and-NH ₂ Can be condensed and combined with triacetyl gallic acid; the carboxymethyl cellulose fiber after acid activation also has better reaction activity and can be combined with triacetyl gallic acid in an esterification way; geraniol is a common natural essence material, has antibacterial and bacteriostatic effects, contains a large amount of hydroxyl, and can be combined with triacetyl gallic acid through esterification. Therefore, the temperature of the molten metal is controlled,in the invention, the alpha-cyclodextrin, the geraniol, the chitosan fiber and the carboxymethyl cellulose fiber can be provided with-OH or-NH ₂ The modification of the carboxymethyl cellulose fiber is completed by condensation reaction with triacetyl gallic acid under heating condition in the presence of p-toluenesulfonic acid as a catalyst.

7. The modified carboxymethyl cellulose fiber belongs to a combined mixture, and combines the properties of chitosan fiber, alpha-cyclodextrin and geraniol, so that the carboxymethyl cellulose fiber has better water absorption and retention capacity and antibacterial capacity, and the strength and toughness of the carboxymethyl cellulose fiber are also better improved. Through detection, the tensile strength of the mask base cloth can reach 2.51MPa, and the bending rigidity can reach 0.70cN cm ² Per cm, the liquid absorption rate is as high as 1815.0%, the liquid retention rate is as high as 86.7%, and the bacteriostatic rate for escherichia coli and staphylococcus aureus is as high as more than 99.9%.

Detailed Description

For the purpose of more clearly illustrating the present invention and more clearly understanding the technical features, objects and advantages of the present invention, the technical solutions of the present invention will now be described in detail below, but are not to be construed as limiting the implementable scope of the present invention.

The invention is further described below with reference to the following examples.

Example 1

A preparation method of a carboxymethyl cellulose fiber facial mask comprises the following steps:

step 1, preparing a mask base cloth:

(1) Dispersing fibers:

mixing carboxymethyl cellulose fibers and chitosan fibers in deionized water, wherein the solid-liquid ratio of the carboxymethyl cellulose fibers to the chitosan fibers to the deionized water is 2.7;

(2) Preparing triacetyl gallic acid:

mixing p-toluenesulfonic acid and acetic anhydride, stirring uniformly, adding dried gallic acid, wherein the weight ratio of the gallic acid to the p-toluenesulfonic acid to the acetic anhydride is 14.3;

(3) Modified carboxymethyl cellulose fiber:

and (2) sequentially adding alpha-cyclodextrin, geraniol and triacetyl gallic acid into the fiber dispersion liquid, wherein the mass ratio of the alpha-cyclodextrin, the geraniol and the triacetyl gallic acid to the fiber dispersion liquid is 1.4.

(4) Modified carboxymethyl cellulose fiber mask base cloth:

dissolving modified carboxymethyl cellulose fiber in N, N-dimethylformamide to form a uniform solution (mass concentration is 50%), forming the uniform solution as a spinning solution, and performing electrostatic spinning technology to set equipment as follows: the temperature is room temperature, the spinning voltage is 30kv, the distance between the needle head and the receiving plate is 20cm, the spinning speed is 2mL/h, and the receiving plate receives the film-forming material and then dries in a drying oven to obtain the mask base cloth;

step 2, preparing facial mask liquid:

mixing the plant extract, the humectant, the thickener, the emulsifier, the pH regulator and deionized water according to a weight ratio of 5;

wherein the plant extract comprises a mixture of a peony root extract, a rheum palmatum extract, a glycyrrhiza glabra extract, a seabuckthorn oil extract and an arbutin extract according to a mass ratio of 1.2; the humectant comprises glycerol, 1,3-propylene glycol, PEG/PPG-17/6 copolymer and sodium hyaluronate, and the mass ratio of the mixture is 0.5; the thickening agent is xanthan gum; the emulsifier comprises sorbitan fatty acid ester and PPG-26-butanol polyether-26 with the mass ratio of 2:1; the preservative is glyceryl caprylate; the pH regulator comprises citric acid and sodium citrate with the mass ratio of 1.

Step 3, preparing the facial mask:

placing the prepared mask liquid in a wide-mouth and clean container, slowly placing the prepared mask base cloth on the surface of the mask liquid after the prepared mask base cloth is unfolded, slowly pressing the prepared mask base cloth into the mask liquid after the surface of the mask liquid is completely unfolded, completely soaking the mask base cloth into the mask liquid, starting an ultrasonic instrument, controlling the ultrasonic temperature to be 35 ℃, the ultrasonic power to be 500W and the ultrasonic time to be 2h, taking out the mask base cloth to be above the mask liquid after the ultrasonic is finished, and folding and packaging the mask base until the speed of the dropped mask liquid is lower than 2 seconds per drop, thereby finishing the preparation of the mask.

Example 2

step 1, preparing a mask base cloth:

(1) Dispersing fibers:

mixing carboxymethyl cellulose fibers and chitosan fibers in deionized water, wherein the solid-liquid ratio of the carboxymethyl cellulose fibers to the chitosan fibers to the deionized water is 1.5;

(2) Preparing triacetyl gallic acid:

mixing p-toluenesulfonic acid and acetic anhydride, stirring uniformly, adding dried gallic acid, wherein the weight ratio of the gallic acid to the p-toluenesulfonic acid to the acetic anhydride is 12.8;

(3) Modified carboxymethyl cellulose fiber:

sequentially adding alpha-cyclodextrin, geraniol and triacetyl gallic acid into a fiber dispersion liquid, wherein the mass ratio of the alpha-cyclodextrin, the geraniol and the triacetyl gallic acid to the fiber dispersion liquid is 1.2.

(4) Modified carboxymethyl cellulose fiber mask base cloth:

dissolving modified carboxymethyl cellulose fiber in N, N-dimethylformamide to form a uniform solution, forming the uniform solution as a spinning solution, and setting equipment into the following steps by an electrostatic spinning technology: the temperature is room temperature, the spinning voltage is 20kv, the distance between the needle head and the receiving plate is 20cm, the spinning speed is 1mL/h, and the receiving plate receives the film-forming material and then dries in a drying oven to obtain the mask base cloth;

step 2, preparing facial mask liquid:

mixing the plant extract, the humectant, the thickener, the emulsifier, the pH regulator and deionized water according to the following weight ratio of 3;

wherein the plant extract comprises a mixture of gallnut extract, scutellaria root extract, cnidium fruit extract, geranium extract and alfalfa extract according to a mass ratio of 1.3; the humectant comprises glycerol, mannitol, glycine, 1,3-propylene glycol which are mixed according to the mass ratio of 1.1; the thickening agent is carbomer; the emulsifier comprises sorbitan fatty acid ester and PEG-40 hydrogenated castor oil in a mass ratio of 1; the preservative is p-hydroxyacetophenone; the pH regulator comprises citric acid and sodium citrate with the mass ratio of 1.

Step 3, preparing the facial mask:

placing the prepared mask liquid in a wide-mouth and clean container, slowly placing the prepared mask base cloth on the surface of the mask liquid after the prepared mask base cloth is unfolded, slowly pressing the prepared mask base cloth into the mask liquid after the surface of the mask liquid is completely unfolded, completely soaking the mask base cloth into the mask liquid, starting an ultrasonic instrument, controlling the ultrasonic temperature to be 25 ℃, the ultrasonic power to be 300W and the ultrasonic time to be 3h, taking out the mask base cloth to be above the mask liquid after the ultrasonic is finished, and folding and packaging the mask base until the speed of the dropped mask liquid is lower than 2 seconds per drop, thereby completing the preparation of the mask.

Example 3

step 1, preparing a mask base cloth:

(1) Dispersing fibers:

mixing carboxymethyl cellulose fibers and chitosan fibers in deionized water, wherein the solid-liquid ratio of the carboxymethyl cellulose fibers, the chitosan fibers and the deionized water is 3;

(2) Preparing triacetyl gallic acid:

mixing p-toluenesulfonic acid and acetic anhydride, uniformly stirring, adding dried gallic acid, wherein the weight ratio of the gallic acid to the p-toluenesulfonic acid to the acetic anhydride is 17.6;

(3) Modified carboxymethyl cellulose fiber:

sequentially adding alpha-cyclodextrin, geraniol and triacetyl gallic acid into a fiber dispersion liquid, wherein the mass ratio of the alpha-cyclodextrin, the geraniol and the triacetyl gallic acid to the fiber dispersion liquid is (1.6).

(4) Modified carboxymethyl cellulose fiber mask base cloth:

dissolving modified carboxymethyl cellulose fiber in N, N-dimethylformamide to form a uniform solution, forming the uniform solution as a spinning solution, and setting equipment into the following steps by an electrostatic spinning technology: the temperature is room temperature, the spinning voltage is 50kv, the distance between the needle head and the receiving plate is 20cm, the spinning speed is 2mL/h, and the receiving plate receives the film-forming material and then dries in a drying oven to obtain the mask base cloth;

step 2, preparing facial mask liquid:

mixing the plant extract, the humectant, the thickener, the emulsifier, the pH regulator and deionized water according to the following weight ratio of 6;

wherein the plant extract comprises a mixture of geranium extract, alfalfa extract, white peony root extract, lily extract and arbutin extract according to a mass ratio of 0.5; the humectant comprises glycerol, 1-3 butanediol, polyethylene glycol, PEG/PPG-17/6 copolymer, and sodium hyaluronate according to the mass ratio of 2.3; the thickening agent is carbomer; the emulsifier is sorbitan fatty acid ester; the preservative is caprylyl hydroximic acid; the pH regulator comprises citric acid and/or sodium citrate with the mass ratio of 1.

Step 3, preparing the facial mask:

placing the prepared mask liquid in a wide-mouth and clean container, slowly placing the prepared mask base cloth on the surface of the mask liquid after the prepared mask base cloth is unfolded, slowly pressing the prepared mask base cloth into the mask liquid after the surface of the mask liquid is completely unfolded, completely soaking the mask base cloth into the mask liquid, starting an ultrasonic instrument, controlling the ultrasonic temperature to be 45 ℃, the ultrasonic power to be 800W and the ultrasonic time to be 0.5h, taking out the mask base cloth to be above the mask liquid after the ultrasonic is finished, and folding and packaging the mask base until the speed of the dropped mask liquid is lower than 2 seconds per drop, thereby finishing the preparation of the mask.

Example 4

The preparation method of the carboxymethyl cellulose fiber facial mask is different from the preparation method of the example 1 in two points: firstly, the mass ratio of carboxymethyl cellulose fiber to chitosan fiber is different; secondly, the proportion of the alpha-cyclodextrin, the geraniol and the triacetyl gallic acid is adjusted.

The method specifically comprises the following steps:

step 1, preparing a mask base cloth:

(1) Dispersing fibers:

mixing carboxymethyl cellulose fibers and chitosan fibers in deionized water, wherein the solid-liquid ratio of the carboxymethyl cellulose fibers to the chitosan fibers to the deionized water is 3.5;

(2) Preparing triacetyl gallic acid:

(3) Modified carboxymethyl cellulose fiber:

(4) Modified carboxymethyl cellulose fiber mask base cloth:

dissolving modified carboxymethyl cellulose fiber in N, N-dimethylformamide to form a uniform solution, forming the uniform solution as a spinning solution, and setting equipment into the following steps by an electrostatic spinning technology: the temperature is room temperature, the spinning voltage is 30kv, the distance between the needle head and the receiving plate is 20cm, the spinning speed is 2mL/h, and the receiving plate receives the film-forming material and then dries in a drying oven to obtain the mask base cloth;

step 2, preparing facial mask liquid:

Step 3, preparing the facial mask:

Example 5

The method specifically comprises the following steps:

step 1, preparing a mask base cloth:

(1) Dispersing fibers:

mixing carboxymethyl cellulose fibers and chitosan fibers in deionized water, wherein the solid-liquid ratio of the carboxymethyl cellulose fibers, the chitosan fibers and the deionized water is 1;

(2) Preparing triacetyl gallic acid:

(3) Modified carboxymethyl cellulose fiber:

sequentially adding alpha-cyclodextrin, geraniol and triacetyl gallic acid into a fiber dispersion liquid, wherein the mass ratio of the alpha-cyclodextrin, the geraniol and the triacetyl gallic acid to the fiber dispersion liquid is 1.6.

(4) Modified carboxymethyl cellulose fiber mask base cloth:

step 2, preparing facial mask liquid:

mixing the plant extract, the humectant, the thickener, the emulsifier, the pH regulator and deionized water according to the following weight ratio of (5);

Step 3, preparing the facial mask:

Comparative example 1

A carboxymethyl cellulose fiber mask base cloth is prepared by the preparation method of example 1, and the difference is that:

the steps of (2) preparing triacetyl gallic acid and (3) modifying carboxymethyl cellulose fiber are omitted, namely, (1) dispersing fiber is obtained to obtain fiber dispersion liquid which is used as spinning liquid to carry out electrostatic spinning, and the electrostatic spinning technology is the same as that of the example 1.

Namely: (1) dispersed fibers:

(2) Carboxymethyl cellulose fiber mask base cloth:

taking the fiber dispersion liquid as spinning liquid, and adopting an electrostatic spinning technology to set the equipment as follows: the temperature is room temperature, the spinning voltage is 30kv, the distance between a needle head and a receiving plate is 20cm, and the receiving plate receives the film-forming material and then dries in a drying oven to obtain the mask base cloth.

Comparative example 2

the step of (2) preparing triacetyl gallic acid is omitted, and the step of (3) modifying carboxymethyl cellulose fiber is adjusted, and the propyl gallate is added instead of the alpha-cyclodextrin, the geraniol and the triacetyl gallic acid. Namely:

(1) Dispersing fibers:

(2) Carboxymethyl cellulose fiber mask base cloth:

putting propyl gallate into the fiber dispersion liquid, stirring to form a uniform solution, wherein the adding amount of the propyl gallate is 1/5 of the total mass of the fiber dispersion liquid, and the propyl gallate is used as a spinning solution, and through an electrostatic spinning technology, the equipment is set as follows: the temperature is room temperature, the spinning voltage is 30kv, the distance between the needle head and the receiving plate is 20cm, and the receiving plate receives the film-forming material and then dries in a drying oven to obtain the mask base cloth.

Comparative example 3

A carboxymethyl cellulose fiber mask base fabric prepared by the preparation method of example 1, with the difference that:

the step of (2) preparing triacetyl gallic acid is omitted, and the step of (3) modifying carboxymethyl cellulose fiber is adjusted, and geraniol and triacetyl gallic acid are not added, but alpha-cyclodextrin is added. Namely:

(1) Dispersing fibers:

(2) Carboxymethyl cellulose fiber mask base cloth:

adding alpha-cyclodextrin into the fiber dispersion liquid, stirring to form a uniform solution, wherein the adding amount of the alpha-cyclodextrin is 1/5 of the total mass of the fiber dispersion liquid, taking the alpha-cyclodextrin as spinning liquid, and performing electrostatic spinning technology, wherein the equipment is set as follows: the temperature is room temperature, the spinning voltage is 30kv, the distance between the needle head and the receiving plate is 20cm, and the receiving plate receives the film-forming material and then dries in a drying oven to obtain the mask base cloth.

Comparative example 4

the step of (2) preparing triacetyl gallic acid is omitted, and the step of (3) modifying carboxymethyl cellulose fiber is adjusted, and the geraniol and the triacetyl gallic acid are not added, but the alpha-cyclodextrin and the propyl gallate are added. Namely:

(1) Dispersing fibers:

(2) Carboxymethyl cellulose fiber mask base cloth:

adding alpha-cyclodextrin and propyl gallate into the fiber dispersion liquid, stirring to form a uniform solution, wherein the addition amount of the alpha-cyclodextrin and the propyl gallate is 1/10 of the total mass of the fiber dispersion liquid respectively, and the alpha-cyclodextrin and the propyl gallate are used as spinning solutions, and the equipment is set as follows through an electrostatic spinning technology: the temperature is room temperature, the spinning voltage is 30kv, the distance between the needle head and the receiving plate is 20cm, and the receiving plate receives the film-forming material and then dries in a drying oven to obtain the mask base cloth.

And (3) experimental detection:

the mask base cloth prepared by the methods of example 1, example 4 and example 5 and comparative examples 1 to 4 is tested for performance, and the performance evaluation of the mask base cloth mainly comprises the performance evaluation of the thickness, the tensile property, the bending performance, the air and moisture permeability, the moisture absorption and retention property and the antibacterial activity, and the specific performance evaluation refers to the performance test and evaluation of the fiber base mask in the prior art.

1. Tensile property:

the tensile strength of the wet film in the longitudinal and transverse directions was measured by an electronic stretching apparatus after the samples were immersed in deionized water for 1min, taken out after being suspended and left standing for 2min under standard atmospheric conditions (20. + -. 2 ℃ C., 65. + -.5% RH), and the average value was obtained by placing the wet film between two clamps of the stretching apparatus (100 mm) at a stretching speed of 100. + -.10 mm/min and calculating the strength per unit area = strength/(width. Multidot. Thickness).

2. Bending property:

three samples of 5cm × 5cm size were cut out under standard atmospheric conditions (20. + -. 2 ℃ C., 65. + -. 5% RH), and the bending stiffness of the samples in the longitudinal and transverse directions in a wet state was measured by a KES-FB2 pure bending tester, and the average value was obtained.

3. Air permeability and moisture permeability:

according to GB/T4218.15-2018, the permeability of the sample is tested by a YG461E digital permeability instrument under standard atmospheric conditions (20 +2 ℃, 65+5% RH), the pressure drop is 50Pa, and the test area is 20cm ² And testing different parts for three times, and taking an average value.

The moisture permeability of the membrane cloth was tested according to GB/T2704.1-2009 under standard atmospheric conditions (20. + -. 2 ℃, 65. + -.5% RH) using a YG601H moisture permeameter using the frontal cup method, and each sample was tested three times and averaged.

4. Moisture absorption and retention performance:

the liquid absorption of the sample was measured according to GB/T24218.6-2010. Due to the limitations of the specimen size structure, the protocol was modified based on the standard: samples of 6.5 cm. Times.6.5 cm size were cut out at 18. + -. 2 ℃ and 45. + -. 3% RH, three samples for each sample. Firstly, weighing a weighing bottle with a bottle stopper to obtain m ₀ After humidifying, weighing the mixture by using a weighing bottle with a bottle stopper to obtain m ₁ . Immersing the sample in deionized water, taking out after 1min, vertically suspending and standing for 2min, putting into a weighing bottle, and weighing to m ₂ Oven drying in 37 constant temperature oven for 20min, taking out, weighing, and recording as m ₃ 。

The liquid absorption rate (LAC) is calculated as follows:

the liquid retention rate (N) is calculated by the following formula:

5. bacteriostasis:

after the mask cloths in examples and comparative examples were dried according to the standard of GB/T20944.3-2007, three samples of 5cm × 5cm size were cut out, each sample was put into a triangular flask of test bacterial liquid of a certain concentration, and oscillated at a predetermined temperature for a certain time, the viable bacterial concentration of the bacterial liquid in the triangular flask before and after oscillation for a certain time was measured, and the bacteriostatic ratio was calculated, thereby evaluating the antibacterial effect of the samples.

The results express: and taking the calculated value of the bacteriostasis rate as a result. When the calculated value of the bacteriostasis rate is negative, the calculated value is expressed as 0; when the calculated value of the bacteriostasis rate is more than or equal to 0, the value is expressed as more than or equal to 0.

The evaluation results are shown in the following table:

as can be seen from the above table, examples 1, 4 and 5 of the present invention performed substantially better than comparative examples 1 to 4 in terms of tensile strength, flexural strength, moisture vapor permeability and moisture absorption and retention. In addition, the antibacterial rate of the composition is higher than 99.9% in the antibacterial aspect of escherichia coli and staphylococcus aureus, which shows that the added substances have effective components with antibacterial enhancement, and the more probable reason is the action of geraniol and triacetyl gallic acid compositions.

Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims

1. The preparation method of the carboxymethyl cellulose fiber facial mask is characterized by comprising the following steps of:

step 1, preparing a mask base cloth:

(1) Dispersing fibers:

(2) Preparing triacetyl gallic acid:

(3) Modified carboxymethyl cellulose fiber:

(4) Modified carboxymethyl cellulose fiber mask base cloth:

step 2, preparing facial mask liquid:

step 3, preparing the facial mask:

2. The preparation method of the carboxymethyl cellulose fiber facial mask according to claim 1, wherein in the step 1 (1), the mass fraction of the acetic acid solution is 15% -20%, and the addition amount of the acetic acid solution is based on the mass content of acetic acid in the final solution being 1%; the temperature in the constant temperature water bath kettle is 45-55 ℃, and the stirring time is 1-2h.

3. The method for preparing a carboxymethyl cellulose fiber mask as claimed in claim 1, wherein in the step (1) of the step 1, the density of carboxymethyl cellulose fiber is 1.2g/cm ³ The deacetylation degree of the chitosan fiber is 90-95%; the solid-liquid ratio (the ratio of solid mass to liquid volume) of the carboxymethyl cellulose fiber, the chitosan fiber and the deionized water is 1-3.

4. The method for preparing a carboxymethyl cellulose fiber mask as claimed in claim 1, wherein in the step (1) of the step 1, the purification is performed by using a dialysis bag purification method, and the cut-off molecular weight is 10000Da; the drying is vacuum drying, the temperature is 50 ℃, and the drying time is 12 hours; the solid-to-liquid ratio of the mixed fiber to the N, N-dimethylformamide is 1:6-10.

5. The method for preparing a carboxymethyl cellulose fiber mask according to claim 1, wherein in the step 1 (2), the weight ratio of gallic acid, p-toluenesulfonic acid and acetic anhydride is 12-17.8-8.6; the temperature of the constant temperature water bath kettle is 60-70 ℃, and the stirring reaction is carried out for 2-3h; the added deionized water is 2 times of the volume of the reaction liquid; ethyl acetate is used for extraction, and the extraction times are three times; the drying is vacuum drying.

6. The method for preparing a carboxymethyl cellulose fiber mask according to claim 1, wherein in the step 1 (3), the mass ratio of α -cyclodextrin, geraniol, triacetyl gallic acid to the fiber dispersion is 1.2-1.6; the catalyst is p-toluenesulfonic acid, and the addition amount of the p-toluenesulfonic acid is 0.2 to 0.8 percent of the mass of the fiber dispersion liquid; heating to 130-160 ℃, and stirring for reaction for 4-6h; the volume of the glacial ethyl ether was 2 times the volume of the reaction solution, and the recrystallization was carried out using a water/ethanol system.

7. The method for preparing a carboxymethyl cellulose fiber mask as claimed in claim 1, wherein in step 1 (4), the electrospinning device is configured as follows: the temperature is room temperature, the spinning voltage is 20-50kv, the distance between the needle head and the receiving plate is 20cm, the spinning speed is 1-2mL/h, and the receiving plate receives the film-forming material and then dries in a drying oven.

8. The preparation method of the carboxymethyl cellulose fiber facial mask according to claim 1, wherein in the step 2, the weight ratio of the plant extract, the humectant, the thickener, the emulsifier, the pH regulator and the deionized water is (3-6).

9. The method for preparing the carboxymethyl cellulose fiber facial mask according to claim 1, wherein in the step 2, the plant extract comprises at least one of a peony root extract, a gallnut extract, a rheum palmatum extract, a scutellaria baicalensis root extract, a cnidium fruit extract, a glycyrrhiza glabra extract, a seabuckthorn oil extract, a geranium extract, a alfalfa extract, a white peony root extract, a lily bulb extract and an arbutin extract; the humectant comprises at least one of glycerol, mannitol, glycine, 1,3-propylene glycol, 1-3 butanediol, polyethylene glycol, PEG/PPG-17/6 copolymer, and sodium hyaluronate; the thickener comprises xanthan gum and/or carbomer; the emulsifier comprises at least one of sorbitan fatty acid ester, PPG-26-butanol polyether-26, and PEG-40 hydrogenated castor oil; the preservative comprises at least one of glyceryl caprylate, p-hydroxyacetophenone and caprylyl hydroxamic acid; the pH regulator comprises citric acid and/or sodium citrate.

10. The preparation method of the carboxymethyl cellulose fiber mask solution according to claim 1, wherein in the step 3, the process of completely soaking the mask base cloth in the mask solution comprises the following steps: placing the prepared facial mask liquid in a wide-mouth and clean container, unfolding the prepared facial mask base cloth, slowly placing the facial mask base cloth on the surface of the facial mask liquid, and slowly pressing the facial mask liquid into the facial mask liquid after the surface of the facial mask liquid is completely unfolded; the ultrasonic treatment is carried out in an ultrasonic instrument, the ultrasonic temperature is 25-45 ℃, the ultrasonic power is 300-800W, and the ultrasonic time is 0.5-3h; and taking out the mask base cloth to the upper part of the mask liquid, and folding and packaging until the speed of the dropped mask liquid is lower than 2 seconds per drop.