A kind of seaweed tencel hydrogel mask cloth and preparation method thereof

Abstract

The invention relates to a seaweed Tencel hydrogel mask cloth and a preparation method thereof, and belongs to the technical field of non-woven fabrics. The mask cloth is formed by spunlacing composite seaweed fibers and Tencel fibers, wherein the composite seaweed fibers are formed by double-terminal unsaturated double bond click addition of octanethiol and diallylamine to form a thioether compound containing secondary amine, i.e., a modifier, and then the modifier is transesterified with propylene glycol alginate at high temperature, and the modifier is grafted onto the macromolecule of propylene glycol alginate, and the nitrogen element in the modifier and the thioether structure form a chelating effect, chelate and adsorb zirconium ions in a liquid phase environment, and zirconium doping is uniformly introduced into the macromolecule of alginate, and seaweed functional particles are formed after pyrolysis and carbonization, and then sodium alginate is used as the main molding material to make fibers, and the seaweed functional particles emit far infrared rays, stimulate the expansion of facial capillaries, promote the opening of pores and blood circulation, and are beneficial to the repair of facial skin by the active ingredients in the essence.

Description

Technical Field

[0001] The invention belongs to the technical field of non-woven fabrics, and in particular, relates to a seaweed Tencel hydrogel mask cloth and a preparation method thereof. Background Art

[0002] With the progress of society and the improvement of living standards, beauty textile materials represented by functions such as beauty, health care, comfort and leisure have shown strong market demand. Facial mask materials in the field of skin care products have developed rapidly. While providing beauty and moisturizing effects, facial mask products have special effects such as eliminating fatigue and relieving stress. They are an important application field of modern textile materials.

[0003] At present, the raw materials used for facial mask cloths on the market are mainly cotton fiber and polyester. In addition, other materials such as silk and chitin fiber are also used in facial mask base cloths. It is precisely because of the diversification of raw materials and processing technology of facial mask base cloths that facial mask base cloths have become rich and diverse, and different facial mask base cloths have great differences in performance and price. Among them, seaweed fiber is a new type of bio-regenerative fiber, which has high hygroscopicity, high oxygen permeability, gel blocking, good biodegradability and compatibility, and is an excellent material for facial mask cloth. Although seaweed fiber facial mask cloth has certain applications in the field of skin care, it mainly focuses on moisturizing and cleaning, and has limited effect on repairing damaged facial skin. Summary of the invention

[0004] In order to solve the technical problems mentioned in the background technology, the object of the present invention is to provide a seaweed Tencel hydrogel mask cloth and a preparation method thereof.

[0005] The purpose of the present invention can be achieved through the following technical solutions:

[0006] A seaweed tencel hydrogel mask cloth is made by spunlacing composite seaweed fibers and tencel fibers, wherein the composite seaweed fibers are prepared by the following method:

[0007] Step A1: Mix diallylamine, octyl mercaptan, dimethylphenylphosphine and ethanol, introduce nitrogen protection, heat to 55-70°C, apply 120-150 rpm stirring and 180-250 W / m 2 UV irradiation, reaction for 2-3.5 hours, after the reaction is completed, ethanol is removed by rotary evaporation to obtain a modifier;

[0008] Furthermore, the dosage ratio of diallylamine, octanethiol, dimethylphenylphosphine and ethanol is 0.1 mol: 0.2 mol: 25-35 mg: 40-60 mL. Under the initiation of ultraviolet radiation, octanethiol and the double-terminal unsaturated double bonds of diallylamine undergo click addition to form a secondary amine-containing thioether compound.

[0009] Step A2: propylene glycol alginate, a modifier, triethylamine and dimethylacetamide are mixed, nitrogen protection is introduced, the temperature is raised to 120-140° C., stirring is applied at 60-90 rpm, reflux reaction is carried out for 5-6 hours, zirconium nitrate solution is added and mixed, the mixture is allowed to stand for 24 hours, centrifuged, the aqueous phase is removed and dried, and then transferred to a pyrolysis furnace, treated at a temperature of 280-320° C. for 6-8 hours under a nitrogen atmosphere, and then pulverized after cooling to obtain seaweed functional particles;

[0010] Furthermore, the dosage ratio of propylene glycol alginate, modifier, zirconium nitrate, triethylamine and dimethylacetamide is 100g:50-70mmol:1.2-1.7g:10-15mL:150-200mL, the mass fraction of zirconium nitrate solution is 1%, the modifier and propylene glycol alginate are transesterified at high temperature, and the modifier is grafted onto the macromolecule of propylene glycol alginate, and its nitrogen and thioether structure form a chelate, which is combined with the added zirconium and carbonized under a pyrolysis environment.

[0011] Step A3: Sodium alginate, polyvinyl alcohol, seaweed functional particles, glycerol and water are mixed, heated to 80-90° C., mixed evenly, vacuum degassed to obtain a spinning solution, and then transferred to a spinning machine, spun into a calcium chloride coagulation bath, and drawn to obtain composite seaweed fibers;

[0012] Furthermore, the dosage ratio of sodium alginate, polyvinyl alcohol, seaweed functional particles, glycerol and water is 10g: 2.8-3.6g: 0.12-0.18g: 0.5-0.7mL: 500mL, and the fibers are made of sodium alginate as the main molding material through wet blending and spinning.

[0013] Furthermore, the linear density of the composite seaweed fiber is 1.6±0.05 dtex.

[0014] A method for preparing a seaweed tencel hydrogel mask cloth comprises the following steps:

[0015] Step S1: the composite seaweed fiber and the tencel fiber are mixed, and the mixture is opened, combed and laid to obtain a grey fabric;

[0016] Step S2: transferring the grey cloth into a spunlace machine for spunlace reinforcement, rolling and dehydrating, and baking and drying to obtain a seaweed Tencel hydrogel mask cloth.

[0017] Furthermore, the mass ratio of the composite seaweed fiber to the tencel fiber is 1:2.5-3.2.

[0018] Furthermore, the water spunlace pressure during the water spunlace reinforcement process is 20-25 MPa.

[0019] Beneficial effects of the present invention:

[0020] The present invention adopts composite seaweed fiber and tencel fiber to prepare the mask cloth, wherein the composite seaweed fiber is formed by the double-terminal unsaturated double bond click addition of octanethiol and diallylamine to form a thioether compound containing secondary amine, i.e., a modifier, and then the modifier is transesterified with propylene glycol alginate at high temperature, and the modifier is grafted onto the macromolecule of propylene glycol alginate, and the nitrogen element in the modifier and the thioether structure form a chelating effect, chelate and adsorb zirconium ions in a liquid environment, and zirconium doping is uniformly introduced into the macromolecule of alginate, and seaweed functional particles are formed after pyrolysis and carbonization. The fibers are made of sodium alginate as the main molding material, which becomes gel-like after absorbing water and has good skin-fitting and moisturizing properties. The seaweed functional particles retain the structure of seaweed carbide and emit a certain amount of far-infrared rays. The uniformly introduced zirconium element forms zirconium oxide with a micro-nano structure after pyrolysis. The study found that it can greatly promote the emission of far-infrared rays. When compounded in the mask cloth, it stimulates the expansion of facial capillaries, promotes the opening of pores and blood circulation, and is beneficial to the repair of facial skin by the active ingredients in the essence. DETAILED DESCRIPTION

[0021] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0022] Example 1, preparation of seaweed Tencel hydrogel mask cloth, the specific implementation process is as follows:

[0023] (1) Preparation of composite seaweed fiber

[0024] Step A1: Mix diallylamine, octyl mercaptan, dimethylphenylphosphine and ethanol, introduce nitrogen protection, heat to 70°C, stir at 150 rpm and apply 250 W / m 2 The mixture was irradiated with ultraviolet light and reacted for 2 hours. After the reaction, ethanol was removed by rotary evaporation to obtain a modifier, wherein the dosage ratio of diallylamine, octanethiol, dimethylphenylphosphine and ethanol was 0.1 mol: 0.2 mol: 35 mg: 60 mL.

[0025] Step A2: Mix propylene glycol alginate, modifier, triethylamine and dimethylacetamide, introduce nitrogen protection, heat to 140°C, stir at 90rpm, reflux for 5h, prepare zirconium nitrate into an aqueous solution with a mass fraction of 1%, add the zirconium nitrate solution and mix, let stand for 24h, centrifuge to separate the liquid, remove the aqueous phase and dry, then transfer to a pyrolysis furnace, treat at 320°C for 6h under a nitrogen atmosphere, and crush after cooling to obtain seaweed functional particles, wherein the amount ratio of propylene glycol alginate, modifier, zirconium nitrate, triethylamine and dimethylacetamide is 100g:70mmol:1.7g:10mL:200mL.

[0026] Step A3: Sodium alginate, polyvinyl alcohol, seaweed functional particles, glycerol and water are mixed, the temperature is raised to 90°C and mixed, vacuum degassing is performed to obtain a spinning solution, and then the solution is transferred to a spinning machine, spun into a calcium chloride coagulation bath, and drawn to form, and the drawn fiber line density is controlled to be 1.6±0.05dtex to obtain a composite seaweed fiber, wherein polyvinyl alcohol is selected from 17-99 type raw materials, the mass fraction of calcium chloride in the calcium chloride coagulation bath is 5%, and the amount ratio of sodium alginate, polyvinyl alcohol, seaweed functional particles, glycerol and water is 10g:2.8g:0.12g:0.7mL:500mL.

[0027] (2) Preparation of facial mask cloth

[0028] Step S1: mixing composite seaweed fiber and Tencel fiber in a mass ratio of 1:2.5, wherein the Tencel fiber is a commercially available short fiber with a specification of 1.3 dtex×38 mm, and performing two steps of opening, carding and laying to obtain a grey cloth;

[0029] Step S2: transferring the grey cloth into the spunlace, controlling the spunlace pressure to 25 MPa, spunlace-reinforce the grey cloth, and then rolling and dehydrating, baking and drying to obtain the seaweed Tencel hydrogel mask cloth.

[0030] Example 2, preparing seaweed Tencel hydrogel mask cloth, the specific implementation process is as follows:

[0031] (1) Preparation of composite seaweed fiber

[0032] Step A1: Mix diallylamine, octyl mercaptan, dimethylphenylphosphine and ethanol, introduce nitrogen protection, heat to 55°C, apply 120 rpm stirring and 180 W / m 2 The mixture was irradiated with ultraviolet light and reacted for 3.5 hours. After the reaction, ethanol was removed by rotary evaporation to obtain a modifier, in which the dosage ratio of diallylamine, octanethiol, dimethylphenylphosphine and ethanol was 0.1 mol: 0.2 mol: 25 mg: 40 mL.

[0033] Step A2: Mix propylene glycol alginate, modifier, triethylamine and dimethylacetamide, introduce nitrogen protection, heat to 120°C, stir at 60rpm, reflux for 6h, prepare zirconium nitrate into an aqueous solution with a mass fraction of 1%, add the zirconium nitrate solution and mix, let stand for 24h, centrifuge to separate the liquid, remove the aqueous phase and dry, then transfer to a pyrolysis furnace, treat at 280°C for 8h under a nitrogen atmosphere, and crush after cooling to obtain seaweed functional particles, wherein the amount ratio of propylene glycol alginate, modifier, zirconium nitrate, triethylamine and dimethylacetamide is 100g:50mmol:1.2g:15mL:150mL.

[0034] Step A3: Sodium alginate, polyvinyl alcohol, seaweed functional particles, glycerol and water are mixed, the temperature is raised to 80°C and mixed, vacuum degassing is performed to obtain a spinning solution, and then the spinning solution is transferred to a spinning machine, spun into a calcium chloride coagulation bath, and drawn to form, and the drawn fiber line density is controlled to be 1.6±0.05dtex to obtain a composite seaweed fiber, wherein polyvinyl alcohol is selected from 17-99 type raw materials, the mass fraction of calcium chloride in the calcium chloride coagulation bath is 5%, and the amount ratio of sodium alginate, polyvinyl alcohol, seaweed functional particles, glycerol and water is 10g:3.6g:0.18g:0.5mL:500mL.

[0035] (2) Preparation of facial mask cloth

[0036] Step S1: the composite seaweed fiber and the Tencel fiber are mixed in a mass ratio of 1:3.2, wherein the Tencel fiber is a commercially available short fiber with a specification of 1.3 dtex×38 mm, and the mixture is opened, combed and laid in two steps to obtain a grey cloth;

[0037] Step S2: transferring the grey cloth into the spunlace, controlling the spunlace pressure to 20 MPa, spunlace-reinforce the grey cloth, and then rolling and dehydrating, baking and drying to obtain the seaweed Tencel hydrogel mask cloth.

[0038] Example 3, preparation of seaweed Tencel hydrogel mask cloth, the specific implementation process is as follows:

[0039] (1) Preparation of composite seaweed fiber

[0040] Step A1: Mix diallylamine, octyl mercaptan, dimethylphenylphosphine and ethanol, introduce nitrogen protection, heat to 60°C, apply 120 rpm stirring and 220 W / m 2 The mixture was irradiated with ultraviolet light and reacted for 3 hours. After the reaction, ethanol was removed by rotary evaporation to obtain a modifier, wherein the dosage ratio of diallylamine, octanethiol, dimethylphenylphosphine and ethanol was 0.1 mol: 0.2 mol: 30 mg: 50 mL.

[0041] Step A2: Mix propylene glycol alginate, modifier, triethylamine and dimethylacetamide, introduce nitrogen protection, heat to 130°C, stir at 60rpm, reflux for 5.5h, prepare zirconium nitrate into an aqueous solution with a mass fraction of 1%, add the zirconium nitrate solution and mix, let stand for 24h, centrifuge to separate the liquid, remove the aqueous phase and dry, then transfer to a pyrolysis furnace, treat at 300°C for 6.5h under a nitrogen atmosphere, and crush after cooling to obtain seaweed functional particles, wherein the amount ratio of propylene glycol alginate, modifier, zirconium nitrate, triethylamine and dimethylacetamide is 100g:60mmol:1.4g:12mL:180mL.

[0042] Step A3: Sodium alginate, polyvinyl alcohol, seaweed functional particles, glycerol and water are mixed, the temperature is raised to 80°C and mixed, vacuum degassing is performed to obtain a spinning solution, and then the spinning solution is transferred to a spinning machine, spun into a calcium chloride coagulation bath, and drawn to form, and the drawn fiber line density is controlled to be 1.6±0.05dtex to obtain a composite seaweed fiber, wherein polyvinyl alcohol is selected from 17-99 type raw materials, the mass fraction of calcium chloride in the calcium chloride coagulation bath is 5%, and the amount ratio of sodium alginate, polyvinyl alcohol, seaweed functional particles, glycerol and water is 10g:3.2g:0.14g:0.6mL:500mL.

[0043] (2) Preparation of facial mask cloth

[0044] Step S1: mixing composite seaweed fiber and Tencel fiber in a mass ratio of 1:3, wherein the Tencel fiber is a commercially available short fiber with a specification of 1.3 dtex×38 mm, and performing two steps of opening, carding and laying to obtain a grey cloth;

[0045] Step S2: transferring the grey cloth into the spunlace, controlling the spunlace pressure to 22 MPa, spunlace-reinforce the grey cloth, and then rolling and dehydrating, baking and drying to obtain the seaweed Tencel hydrogel mask cloth.

[0046] Example 4, preparation of seaweed Tencel hydrogel mask cloth, the specific implementation process is as follows:

[0047] (1) Preparation of composite seaweed fiber

[0048] Step A1: Mix diallylamine, octyl mercaptan, dimethylphenylphosphine and ethanol, introduce nitrogen protection, heat to 65°C, stir at 150 rpm and 220 W / m 2 The mixture was irradiated with ultraviolet light and reacted for 3.2 hours. After the reaction, ethanol was removed by rotary evaporation to obtain a modifier, in which the dosage ratio of diallylamine, octanethiol, dimethylphenylphosphine and ethanol was 0.1 mol: 0.2 mol: 35 mg: 50 mL.

[0049] Step A2: Mix propylene glycol alginate, modifier, triethylamine and dimethylacetamide, introduce nitrogen protection, heat to 135°C, stir at 90rpm, reflux for 5.5h, prepare zirconium nitrate into an aqueous solution with a mass fraction of 1%, add the zirconium nitrate solution and mix, let stand for 24h, centrifuge to separate the liquid, remove the aqueous phase and dry, then transfer to a pyrolysis furnace, treat at 300°C for 7.5h under a nitrogen atmosphere, and crush after cooling to obtain seaweed functional particles, wherein the amount ratio of propylene glycol alginate, modifier, zirconium nitrate, triethylamine and dimethylacetamide is 100g:65mmol:1.5g:12mL:180mL.

[0050] Step A3: Sodium alginate, polyvinyl alcohol, seaweed functional particles, glycerol and water are mixed, the temperature is raised to 85°C and mixed, vacuum degassing is performed to obtain a spinning solution, and then the solution is transferred to a spinning machine, spun into a calcium chloride coagulation bath, and drawn to form, and the drawn fiber line density is controlled to be 1.6±0.05dtex to obtain a composite seaweed fiber, wherein polyvinyl alcohol is selected from 17-99 type raw materials, the mass fraction of calcium chloride in the calcium chloride coagulation bath is 5%, and the amount ratio of sodium alginate, polyvinyl alcohol, seaweed functional particles, glycerol and water is 10g:3.2g:0.16g:0.6mL:500mL.

[0051] (2) Preparation of facial mask cloth

[0052] Step S1: the composite seaweed fiber and the Tencel fiber are mixed in a mass ratio of 1:2.8, wherein the Tencel fiber is a commercially available short fiber with a specification of 1.3 dtex×38 mm, and the mixture is opened, combed and laid in two steps to obtain a grey cloth;

[0053] Step S2: transferring the grey cloth into the spunlace, controlling the spunlace pressure to 22 MPa, spunlace-reinforce the grey cloth, and then rolling and dehydrating, baking and drying to obtain the seaweed Tencel hydrogel mask cloth.

[0054] Comparative Example 1

[0055] This comparative example refers to Example 4, except that no seaweed functional particles are added during the preparation of the composite seaweed fiber, and the rest of the implementation process is exactly the same.

[0056] Comparative Example 2

[0057] This comparative example refers to Example 4, and in the preparation process of the composite seaweed fiber, seaweed charcoal of equal weight is used to replace the seaweed functional particles. At the same time, 2wt% of zirconium oxide powder of the seaweed charcoal is added, and the rest of the implementation process is exactly the same as Example 4; wherein, the preparation method of the seaweed charcoal is: using Sargassum fusiformis as the seaweed raw material, soaking it with water three times, drying it and sieving it to remove the ash, transferring it into a pyrolysis furnace, and carbonizing it at 550°C for 2h under a nitrogen atmosphere, and dry grinding it after cooling to make seaweed charcoal.

[0058] In order to test the relevant properties of the above mask cloth, an essence was prepared: 10wt% glycerol, 0.1wt% hyaluronic acid, 1wt% recombinant human collagen, 0.8wt% bisabolol, 3.5wt% niacinamide, 2.2wt% tranexamic acid, 0.5wt% rose hydrosol, and ultrapure water was added to 100wt%.

[0059] Liquid absorption and liquid retention performance test: cut the above mask cloth and weigh it, recorded as M0, immerse it in essence liquid and let it stand for 10 minutes to fully absorb the liquid, take it out and hang it to stand and drain for 3 minutes, weigh it as M1, take it out and hang it to stand and drain for 6 hours, weigh it as M2, then the liquid absorption rate = (M1-M0) / M0×100%; the liquid retention rate = (M2-M1) / (M1-M0)×100%.

[0060] Moisturizing test: recruit 20 volunteers, expose the back of their hands in a constant temperature room for 30 minutes, apply the above mask that has been left to stand and drain on the back of the volunteers' hands, apply for 15 minutes, and then expose in a constant temperature room for 5 minutes. Use RealBubee skin moisture tester to test the skin moisture, and calculate the hydration rate = (skin moisture after application - skin moisture before application) / skin moisture before application × 100%.

[0061] Skin care test: distribute the mask prepared as above to volunteers, apply it once in the morning and evening, the market cycle is 30 days, and use CBS cloud mirror skin detector to detect the skin condition before and after use;

[0062] Far infrared emissivity test: Take the mask cloth as above and use an IR-2 dual-band emissivity meter to test the far infrared emissivity.

[0063] The specific test results are shown in the following table:

[0064]

[0065]

[0066] It can be seen from the test data in the above table that the seaweed fiber and Tencel composite mask cloth used in the example and the comparative example have good liquid absorption and liquid retention capabilities. Using the same essence, the example has a higher water replenishment rate, and has better effects on lightening shallow pigments, deep pigments and fine lines, and the far-infrared emissivity is about 0.8.

[0067] In the description of the specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0068] The above contents are merely examples and explanations of the present invention. Those skilled in the art may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the invention or exceed the scope defined by the claims, they shall all fall within the protection scope of the present invention.

Claims

1. A seaweed tencel hydrogel mask cloth, which is spunlace-made from composite seaweed fiber and tencel fiber, characterized in that: The composite seaweed fiber is prepared by the following method: Step A1: Mix diallylamine, octyl mercaptan, dimethylphenylphosphine and ethanol, introduce nitrogen protection, heat to 55-70°C, stir and apply 180-250W / m 2 UV irradiation, reaction for 2-3.5h, after the reaction, ethanol is removed by rotary evaporation to obtain a modifier, wherein the amount ratio of diallylamine, octyl mercaptan, dimethylphenylphosphine and ethanol is 0.1mol:0.2mol:25-35mg:40-60mL; Step A2: propylene glycol alginate, a modifier, triethylamine and dimethylacetamide are mixed, nitrogen is introduced for protection, the temperature is raised to 120-140° C., stirring and reflux reaction is carried out for 5-6 hours, and then zirconium nitrate solution is added and mixed, and the mixture is allowed to stand for 24 hours, centrifuged to separate the liquid, the aqueous phase is removed and dried, and then transferred to a pyrolysis furnace, and treated at a temperature of 280-320° C. for 6-8 hours under a nitrogen atmosphere, and then pulverized after cooling to obtain seaweed functional particles, wherein the amount ratio of propylene glycol alginate, modifier, zirconium nitrate, triethylamine and dimethylacetamide is 100 g: 50-70 mmol: 1.2-1.7 g: 10-15 mL: 150-200 mL, and the mass fraction of the zirconium nitrate solution is 1%; Step A3: Mix sodium alginate, polyvinyl alcohol, seaweed functional particles, glycerol and water, heat to 80-90°C and mix evenly, vacuum degassing to obtain a spinning solution, and then transfer it to a spinning machine, spin it into a calcium chloride coagulation bath, and stretch it into shape to obtain a composite seaweed fiber, wherein the amount ratio of sodium alginate, polyvinyl alcohol, seaweed functional particles, glycerol and water is 10g:2.8-3.6g:0.12-0.18g:0.5-0.7mL:500mL.

2. The seaweed Tencel hydrogel mask cloth according to claim 1, characterized in that: The linear density of the composite seaweed fiber is 1.6±0.05dtex.

3. The method for preparing a seaweed Tencel hydrogel mask cloth according to claim 2, characterized in that: The steps include: Step S1: the composite seaweed fiber and the tencel fiber are mixed, and the mixture is opened, combed and laid to obtain a grey fabric; Step S2: transferring the grey cloth into a spunlace machine for spunlace reinforcement, rolling and dehydrating, and baking and drying to obtain a seaweed Tencel hydrogel mask cloth.

4. The method for preparing a seaweed Tencel hydrogel mask cloth according to claim 3, characterized in that: The mass ratio of the composite seaweed fiber to the tencel fiber is 1:2.5-3.

2.

5. The method for preparing a seaweed Tencel hydrogel mask cloth according to claim 4, characterized in that: The water spunlace pressure during the water spunlace reinforcement process is 20-25MPa.

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