CN118600573B - A lavender and valerian modified plant-based fiber and preparation method thereof - Google Patents
A lavender and valerian modified plant-based fiber and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
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- D01F1/00—General methods for the manufacture of artificial filaments or the like
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Abstract
The application relates to the technical field of functional fiber preparation, and in particular discloses a lavender and valerian modified plant-based fiber and a preparation method thereof, wherein the modified plant-based fiber is prepared by the following steps of cleaning, airing and crushing lavender and valerian to obtain plant powder, and extracting the plant powder serving as a raw material to obtain a plant extract; adding the nano graphene sheets into the hydrolysate of the silane coupling agent, adding the plant extract, performing ultrasonic dispersion treatment, adding the sodium alginate coating liquid, fully stirring and mixing, and drying and curing to obtain the functional filler; the modified plant-based fiber prepared by the preparation method can obviously improve the health-care performance and antibacterial and anti-inflammatory performance of the fiber and increase the moisture absorption and air permeability of the fiber while ensuring excellent mechanical performance and thermal stability.
Description
Technical Field
The application relates to the technical field of functional fiber preparation, in particular to a lavender and valerian modified plant-based fiber and a preparation method thereof.
Background
Regenerated cellulose fibers are fibers prepared by chemical treatment and modification of cellulose extracted from nature, and among the most common are bamboo fibers, chitin fibers, lyocell fibers, modal fibers and the like. The regenerated cellulose fiber combines the advantages of natural fiber and synthetic fiber, has wide application in textile industry, and is used for producing various clothes, household articles, industrial products and the like. They are popular with consumers for their good hygroscopicity, breathability and soft feel, and have potential for environmental protection and sustainability.
Regenerated cellulose fibers are commonly used as filling materials in the fields of furniture, infant products, toys, sleeping products, and the like. For example, lyocell fiber can be used as a filler for pillows and quilts because it has good air permeability and hygroscopicity. The pillow core filled with the lyocell fiber can provide moderate neck support, is beneficial to relieving cervical vertebra fatigue, can maintain the shape for a long time, and is not easy to deform. Although regenerated cellulose fiber has some advantages in the aspect of filling the pillow, the regenerated cellulose fiber has poor durability, and long-term use is easy to cause moisture and heat accumulation in the pillow, and meanwhile, the regenerated cellulose fiber is extremely easy to cause problems of peculiar smell, mold growth and the like in the pillow, so that the regenerated cellulose fiber needs to be frequently replaced and used.
Along with the improvement of the living standard of people, the requirements of consumers on the health care and the functionality of bedding are higher and higher. In order to further enhance the overall properties of regenerated cellulose fibers, modified plant-based fibers have been studied and applied. The modified plant-based fiber generally adopts a natural plant extract as a modifier or an additive, and the regenerated cellulose fiber is subjected to dipping treatment after the plant extract is prepared into a treatment liquid, so that the regenerated cellulose fiber is endowed with more excellent antibacterial property, comfort, health care property and the like. However, although the above-mentioned treatment liquid impregnation treatment method can improve the bacteriostasis and comfort of the regenerated cellulose fiber to some extent, the modification effect is not durable. Based on the above statements, the present application provides a lavender, valerian modified plant based fiber and method of making the same.
Disclosure of Invention
In order to improve the health care performance and the functionality of the regenerated cellulose fiber and prolong the modification effect, the application provides a lavender and valerian modified plant-based fiber and a preparation method thereof.
In a first aspect, the application provides a preparation method of lavender and valerian modified plant-based fiber, which adopts the following technical scheme:
a preparation method of lavender and valerian modified plant-based fiber comprises the following preparation steps:
s1, preparing a plant extract:
Washing, airing and crushing lavender and valerian to obtain plant powder, and extracting the plant powder serving as a raw material to obtain a plant extract;
s2, preparing functional filler:
adding the nano graphene sheets into the hydrolysate of the silane coupling agent, adding the plant extract, performing ultrasonic dispersion treatment, adding the sodium alginate coating liquid, fully stirring and mixing, and drying and curing to obtain the functional filler;
S3, preparing modified plant-based fibers:
and (3) blending the cellulose solution, the functional filler, the epoxidized soybean oil and the stearate, and then carrying out wet spinning to obtain the required modified plant-based fiber.
Preferably, the extraction treatment in the step S1 is specifically divided into two times, firstly, the plant powder is primarily extracted by adopting a steam distillation method to collect the extract I, then the plant powder is ultrasonically extracted by adding an ethanol water solution according to the mass ratio of 1:8-12, the filter residue is removed by filtration to obtain the extract II, and the extract I and the extract II are combined to obtain the plant extract.
Preferably, the silane coupling agent hydrolysate in the step S2 is prepared by controlling the mass ratio to be 1:20-24, adding the silane coupling agent into an ethanol water solution, and carrying out hydrolysis reaction for 1-2h at the temperature of 50-60 ℃ to obtain the silane coupling agent hydrolysate.
Preferably, the silane coupling agent is gamma-glycidol ether oxypropyl trimethoxysilane and/or N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane.
Preferably, the sodium alginate coating liquid in the step S2 is prepared by controlling the mass ratio of sodium alginate to stabilizer to water to be 5-6:2-3:22, adding water into sodium alginate, stirring until the sodium alginate is completely dissolved, adding stabilizer, and continuously stirring until the sodium alginate is completely dissolved to obtain the sodium alginate coating liquid.
Preferably, the stabilizer comprises sophorolipid and polyethylene glycol in a mass ratio of 3-5:1.
Preferably, in the step S3, the raw materials comprise, by weight, 80-100 parts of a cellulose solution, 20-30 parts of a functional filler, 3-8 parts of epoxidized soybean oil and 1-3 parts of stearate.
Preferably, the cellulose solution is obtained by dissolving cellulose pulp in an aqueous solution of N-methylmorpholine-N-oxide.
Preferably, the wet spinning in the step S3 specifically comprises the steps of spinning the blend solution at the temperature of 70-90 ℃ through a spinning machine, solidifying the blend solution by taking acetic acid aqueous solution with the temperature of 20-25 ℃ and the mass concentration of 33-38% as solidifying liquid, drafting the blend solution at the drafting multiple of 2-3 times, washing the blend solution by ethanol, and drying the blend solution at the temperature of 40-60 ℃.
In a second aspect, the application provides a lavender and valerian modified plant-based fiber, which adopts the following technical scheme:
the lavender and valerian modified plant-based fiber is prepared by the preparation method of the lavender and valerian modified plant-based fiber.
In summary, the application has the following beneficial effects:
1. The lavender and valerian have obvious effects of calming and hypnotizing, relaxing and soothing, tranquilizing, inhibiting bacteria and diminishing inflammation and the like, and different active ingredients can be effectively extracted by adopting a double extraction means of steam extraction and solvent extraction, so that the extraction spectrum is enlarged, the extraction efficiency is improved, and the effect and quality of a product are improved.
2. According to the application, sophorolipid and polyethylene glycol are compounded to prepare the stabilizer, and the stabilizer is added into the sodium alginate solution to prepare the sodium alginate coating liquid, so that on one hand, the addition of the stabilizer can change the interaction force between gel particles, increase the viscosity and viscoelasticity of sodium alginate gel, enable the gel to form a stable coating layer, slow down the diffusion rate of active substances, and on the other hand, the stabilizer can also interact with the active substances to form a composite structure to provide additional protection, further slow down the release of the active substances and protect the active substances from the influence and degradation of external environment.
3. The preparation method of the modified fiber has the advantages that the plant extracts are fully adsorbed by the nano graphene sheets, the high specific surface area of the nano graphene sheets and the natural oxidation resistance of the plant extracts can be effectively prevented from being degraded due to the influence of external environment, a stable coating layer is formed on the surface of the nano graphene sheets by utilizing sodium alginate coating liquid, on one hand, the premature release of the active ingredients can be effectively prevented by the aid of the structure of sodium alginate gel, the release rate of the active ingredients is delayed, on the other hand, the crosslinking effect among sodium alginate molecules can be improved, the crosslinking density of final fibers can be increased, the mechanical properties and the moisture absorption and ventilation properties of fiber products are improved, and the prepared functional filler can enhance the health-care properties, the antibacterial and anti-inflammatory properties of the fibers and the moisture absorption and ventilation properties of the fibers while enhancing the mechanical properties and the thermal stability of the modified fibers.
Detailed Description
In order that the embodiments of the application may be more readily understood, the application will be described in detail with reference to the following examples, which are intended to be illustrative only and are not limiting of the scope of the application.
Example 1
The lavender and valerian modified plant-based fiber is prepared by the following preparation method:
s1, preparing a plant extract:
collecting fresh lavender and valerian, cleaning, airing, crushing, sieving with a 80-mesh sieve, mixing the lavender powder and the valerian powder according to a mass ratio of 1:3 to obtain plant powder, primarily extracting the plant powder by a steam distillation method for 2 hours to collect an extract I, then adding an ethanol water solution with a mass concentration of 55% into the plant powder according to a mass ratio of 1:8, performing ultrasonic extraction, controlling the ultrasonic temperature to be 50 ℃, the ultrasonic power to be 280W, performing ultrasonic extraction for 2 hours at an ultrasonic frequency of 40kHz, filtering to remove filter residues to obtain an extract II, and combining the extract I and the extract II to obtain a plant extract;
s2, preparing functional filler:
S21, controlling the mass ratio to be 1:20, adding a silane coupling agent into an ethanol water solution with the mass fraction of 65%, and carrying out hydrolysis reaction for 2 hours at the temperature of 50 ℃ to obtain a silane coupling agent hydrolysate, wherein the silane coupling agent comprises gamma-glycidol ether oxypropyl trimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane with the mass ratio of 1:3;
s22, controlling the mass ratio of sodium alginate to stabilizer to water to be 5:2:22, adding water into sodium alginate, stirring at normal temperature until the sodium alginate is completely dissolved, adding stabilizer, continuously stirring until the sodium alginate is completely dissolved, and obtaining sodium alginate coating liquid, wherein the stabilizer comprises sophorolipid and polyethylene glycol 200 in a mass ratio of 3:1;
S23, adding nano graphene sheets (the thickness is 4-20nm, the diameter is 5-10 mu m, the density is 0.23g/cm 3) into a silane coupling agent hydrolysate, controlling the stirring rotation speed to be 350r/min, stirring at 50 ℃ for 2 hours, adding a plant extract, controlling the ultrasonic temperature to be 50 ℃, the ultrasonic power to be 280W, the ultrasonic frequency to be 40kHz, performing ultrasonic dispersion treatment for 2 hours, finally adding a sodium alginate coating solution, continuously stirring and mixing for 2 hours, and drying and curing at the temperature of 80 ℃ to obtain a functional filler, wherein the mass ratio of the nano graphene sheets, the silane coupling agent hydrolysate, the plant extract and the sodium alginate coating solution is 4:18:1:10;
S3, preparing modified plant-based fibers:
s31, adding pine pulp with the solid content of 50% into boiling slurry according to the mass ratio of 1:4, boiling for 2 hours, filtering, immersing filter residues into sodium hypochlorite solution with the mass concentration of 22%, stirring for 1 hour at the temperature of 60 ℃, filtering, washing the filter residues, and drying to obtain cellulose pulp, wherein the boiling slurry is prepared by mixing sodium hydroxide, sodium sulfite and water according to the mass ratio of 1:3:18;
s32, adding cellulose pulp into an N-methylmorpholine-N-oxide aqueous solution with the mass concentration of 55% according to the mass ratio of 1:6, and stirring at the temperature of 100 ℃ until the cellulose pulp is completely dissolved to obtain a cellulose solution;
S33, mixing 80 parts by weight of cellulose solution, 20 parts by weight of functional filler, 3 parts by weight of epoxidized soybean oil and 1 part by weight of potassium stearate for 40min at a rotating speed of 350r/min, spinning the blend solution at a temperature of 70 ℃ through a spinning machine, curing by taking an acetic acid aqueous solution with a mass concentration of 38% at a temperature of 20 ℃ as a curing solution, drafting by a drafting multiple of 2, washing with ethanol, and drying at a temperature of 60 ℃ to obtain the modified plant-based fiber with a fineness of 2.2 dtex.
Example 2
The lavender and valerian modified plant-based fiber is prepared by the following preparation method:
s1, preparing a plant extract:
Collecting fresh lavender and valerian, cleaning, airing, crushing, sieving with a 80-mesh sieve, mixing the lavender powder and the valerian powder according to a mass ratio of 1:2 to obtain plant powder, primarily extracting the plant powder by a steam distillation method for 2.5h to collect an extract I, then adding an ethanol aqueous solution with a mass concentration of 60% into the plant powder according to a mass ratio of 1:9, performing ultrasonic extraction, controlling the ultrasonic temperature to be 50 ℃, controlling the ultrasonic power to be 300W, performing ultrasonic extraction for 1.8h at an ultrasonic frequency of 42kHz, filtering to remove filter residues to obtain an extract II, and combining the extract I and the extract II to obtain a plant extract;
s2, preparing functional filler:
S21, controlling the mass ratio to be 1:21, adding a silane coupling agent into an ethanol water solution with the mass fraction of 68%, and carrying out hydrolysis reaction for 1.8 hours at the temperature of 52 ℃ to obtain a silane coupling agent hydrolysate, wherein the silane coupling agent comprises gamma-glycidol ether oxypropyl trimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane with the mass ratio of 1:2;
S22, controlling the mass ratio of sodium alginate to stabilizer to water to be 5:3:22, adding water into sodium alginate, stirring at normal temperature until the sodium alginate is completely dissolved, adding stabilizer, continuously stirring until the sodium alginate is completely dissolved, and obtaining sodium alginate coating liquid, wherein the stabilizer comprises sophorolipid and polyethylene glycol 200 in a mass ratio of 3.5:1;
S23, adding nano graphene sheets (the thickness is 4-20nm, the diameter is 5-10 mu m, the number of layers is <30, the density is 0.23g/cm 3) into a silane coupling agent hydrolysate, controlling the stirring speed to be 380r/min, stirring at 52 ℃ for 1.8 hours, adding a plant extract, controlling the ultrasonic temperature to be 50 ℃, controlling the ultrasonic power to be 300W, the ultrasonic frequency to be 42kHz, performing ultrasonic dispersion for 1.8 hours, finally adding a sodium alginate coating liquid, continuously stirring and mixing for 1.2 hours, and drying and curing at 80 ℃ to obtain a functional filler, wherein the mass ratio of the nano graphene sheets to the silane coupling agent hydrolysate to the plant extract to the sodium alginate coating liquid is 6:18:1:10;
S3, preparing modified plant-based fibers:
S31, adding pine pulp with the solid content of 50% into boiling slurry according to the mass ratio of 1:4.2, boiling for 2 hours, filtering, immersing filter residues into sodium hypochlorite solution with the mass concentration of 22%, stirring for 1 hour at the temperature of 60 ℃, filtering, washing the filter residues, and drying to obtain cellulose pulp, wherein the boiling slurry is prepared by mixing sodium hydroxide, sodium sulfite and water according to the mass ratio of 1:3.2:18;
S32, adding cellulose pulp into an N-methylmorpholine-N-oxide aqueous solution with the mass concentration of 58% according to the mass ratio of 1:6.5, and stirring at the temperature of 98 ℃ until the cellulose pulp is completely dissolved to obtain a cellulose solution;
S33, mixing 85 parts by weight of cellulose solution, 22 parts by weight of functional filler, 4 parts by weight of epoxidized soybean oil and 1.5 parts by weight of potassium stearate at a rotating speed of 380r/min for 38min, spinning the blend solution at a temperature of 75 ℃ through a spinning machine, curing by taking an acetic acid aqueous solution with a mass concentration of 36% at a temperature of 21 ℃ as a curing solution, drafting by a drafting multiple of 2.2, washing with ethanol, and drying at a temperature of 55 ℃ to obtain the modified plant-based fiber with a fineness of 2.7 dtex.
Example 3
The lavender and valerian modified plant-based fiber is prepared by the following preparation method:
s1, preparing a plant extract:
Collecting fresh lavender and valerian, cleaning, airing, crushing, sieving with a 80-mesh sieve, mixing the lavender powder and the valerian powder according to a mass ratio of 1:1 to obtain plant powder, primarily extracting the plant powder by a steam distillation method for 3 hours to collect an extract I, then adding an ethanol aqueous solution with a mass concentration of 65% into the plant powder according to a mass ratio of 1:10, performing ultrasonic extraction, controlling the ultrasonic temperature to be 50 ℃, the ultrasonic power to be 310W, performing ultrasonic extraction for 1.5 hours at an ultrasonic frequency of 45kHz, filtering to remove filter residues to obtain an extract II, and combining the extract I and the extract II to obtain a plant extract;
s2, preparing functional filler:
s21, controlling the mass ratio to be 1:22, adding a silane coupling agent into an ethanol water solution with the mass fraction of 70%, and carrying out hydrolysis reaction for 1.5 hours at the temperature of 55 ℃ to obtain a silane coupling agent hydrolysate, wherein the silane coupling agent comprises gamma-glycidol ether oxypropyl trimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane with the mass ratio of 1:1;
s22, controlling the mass ratio of sodium alginate to stabilizer to water to be 6:2:22, adding water into sodium alginate, stirring at normal temperature until the sodium alginate is completely dissolved, adding stabilizer, continuously stirring until the sodium alginate is completely dissolved, and obtaining sodium alginate coating liquid, wherein the stabilizer comprises sophorolipid and polyethylene glycol 400 in a mass ratio of 4:1;
S23, adding nano graphene sheets (the thickness is 4-20nm, the diameter is 5-10 mu m, the number of layers is <30, the density is 0.23g/cm 3) into a silane coupling agent hydrolysate, controlling the stirring speed to be 400r/min, stirring at the temperature of 55 ℃ for 1.5 hours, adding a plant extract, controlling the ultrasonic temperature to be 50 ℃, controlling the ultrasonic power to be 310W, the ultrasonic frequency to be 45kHz, performing ultrasonic dispersion treatment for 1.5 hours, finally adding a sodium alginate coating liquid, continuously stirring and mixing for 1.5 hours, and drying and curing at the temperature of 80 ℃ to obtain a functional filler, wherein the mass ratio of the nano graphene sheets, the silane coupling agent hydrolysate, the plant extract and the sodium alginate coating liquid is 5:19:1:11;
S3, preparing modified plant-based fibers:
S31, adding pine pulp with the solid content of 50% into boiling slurry according to the mass ratio of 1:4.5, boiling for 2 hours, filtering, immersing filter residues into sodium hypochlorite solution with the mass concentration of 22%, stirring for 1 hour at the temperature of 60 ℃, filtering, washing the filter residues, and drying to obtain cellulose pulp, wherein the boiling slurry is prepared by mixing sodium hydroxide, sodium sulfite and water according to the mass ratio of 1:3.5:18;
S32, adding cellulose pulp into an N-methylmorpholine-N-oxide aqueous solution with the mass concentration of 60% according to the mass ratio of 1:7, and stirring at the temperature of 95 ℃ until the cellulose pulp is completely dissolved to obtain a cellulose solution;
S33, mixing 90 parts by weight of cellulose solution, 25 parts by weight of functional filler, 5 parts by weight of epoxidized soybean oil and 2 parts by weight of potassium stearate for 35 minutes at a rotating speed of 400r/min, spinning the blend solution at 80 ℃ through a spinning machine, curing by taking an acetic acid aqueous solution with the temperature of 23 ℃ and the mass concentration of 35% as a curing solution, drafting by a drafting multiple of 2.5 times, washing with ethanol, and drying at the temperature of 50 ℃ to obtain the modified plant-based fiber with the fineness of 2.9 dtex.
Example 4
The lavender and valerian modified plant-based fiber is prepared by the following preparation method:
s1, preparing a plant extract:
collecting fresh lavender and valerian, cleaning, airing, crushing, sieving with a 80-mesh sieve, mixing the lavender powder and the valerian powder according to a mass ratio of 2:1 to obtain plant powder, primarily extracting the plant powder by a steam distillation method for 3.5h to collect an extract I, then adding an ethanol aqueous solution with a mass concentration of 70% into the plant powder according to a mass ratio of 1:11, performing ultrasonic extraction, controlling the ultrasonic temperature to be 50 ℃, controlling the ultrasonic power to be 320W, performing ultrasonic extraction for 1.2h at an ultrasonic frequency of 48kHz, filtering to remove filter residues to obtain an extract II, and combining the extract I and the extract II to obtain a plant extract;
s2, preparing functional filler:
s21, controlling the mass ratio to be 1:23, adding a silane coupling agent into an ethanol water solution with the mass fraction of 72%, and carrying out hydrolysis reaction for 1.2 hours at the temperature of 58 ℃ to obtain a silane coupling agent hydrolysate, wherein the silane coupling agent comprises gamma-glycidol ether oxypropyl trimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane with the mass ratio of 2:1;
S22, controlling the mass ratio of sodium alginate to stabilizer to water to be 6:3:22, adding water into sodium alginate, stirring at normal temperature until the sodium alginate is completely dissolved, adding stabilizer, continuously stirring until the sodium alginate is completely dissolved, and obtaining sodium alginate coating liquid, wherein the stabilizer comprises sophorolipid and polyethylene glycol 400 in a mass ratio of 4.5:1;
S23, adding nano graphene sheets (the thickness is 4-20nm, the diameter is 5-10 mu m, the number of layers is <30, the density is 0.23g/cm 3) into a silane coupling agent hydrolysate, controlling the stirring rotation speed to be 420r/min, stirring at 58 ℃ for 1.2 hours, adding a plant extract, controlling the ultrasonic temperature to be 50 ℃, controlling the ultrasonic power to be 320W, the ultrasonic frequency to be 48kHz, performing ultrasonic dispersion treatment for 1.2 hours, finally adding a sodium alginate coating liquid, continuously stirring and mixing for 1.8 hours, and drying and curing at 80 ℃ to obtain a functional filler, wherein the mass ratio of the nano graphene sheets to the silane coupling agent hydrolysate to the plant extract to the sodium alginate coating liquid is 6:18:1:12;
S3, preparing modified plant-based fibers:
s31, adding pine pulp with the solid content of 50% into boiling slurry according to the mass ratio of 1:4.8, boiling for 2 hours, filtering, immersing filter residues into sodium hypochlorite solution with the mass concentration of 22%, stirring for 1 hour at the temperature of 60 ℃, filtering, washing the filter residues, and drying to obtain cellulose pulp, wherein the boiling slurry is prepared by mixing sodium hydroxide, sodium sulfite and water according to the mass ratio of 1:3.8:18;
S32, adding cellulose pulp into an N-methylmorpholine-N-oxide aqueous solution with the mass concentration of 62% according to the mass ratio of 1:7.5, and stirring at the temperature of 98 ℃ until the cellulose pulp is completely dissolved to obtain a cellulose solution;
s33, mixing 95 parts by weight of cellulose solution, 28 parts by weight of functional filler, 7 parts by weight of epoxidized soybean oil and 2.5 parts by weight of potassium stearate for 32 minutes at a rotating speed of 420r/min, spinning the blend solution at a temperature of 85 ℃ through a spinning machine, curing by taking an aqueous solution of acetic acid with a mass concentration of 34% at a temperature of 24 ℃ as a curing solution, drafting by a drafting multiple of 2.8 times, washing with ethanol, and drying at a temperature of 55 ℃ to obtain the modified plant-based fiber with a fineness of 1.9 dtex.
Example 5
The lavender and valerian modified plant-based fiber is prepared by the following preparation method:
s1, preparing a plant extract:
Collecting fresh lavender and valerian, cleaning, airing, crushing, sieving with a 80-mesh sieve, mixing the lavender powder and the valerian powder according to a mass ratio of 3:1 to obtain plant powder, primarily extracting the plant powder by a steam distillation method for 4 hours to collect an extract I, then adding an ethanol aqueous solution with a mass concentration of 75% into the plant powder according to a mass ratio of 1:12, performing ultrasonic extraction, controlling the ultrasonic temperature to be 50 ℃, controlling the ultrasonic power to be 340W, performing ultrasonic extraction for 1 hour at an ultrasonic frequency of 50kHz, filtering to remove filter residues to obtain an extract II, and combining the extract I and the extract II to obtain a plant extract;
s2, preparing functional filler:
S21, controlling the mass ratio to be 1:24, adding a silane coupling agent into an ethanol water solution with the mass fraction of 75%, and carrying out hydrolysis reaction for 1h at the temperature of 60 ℃ to obtain a silane coupling agent hydrolysate, wherein the silane coupling agent comprises gamma-glycidol ether oxypropyl trimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane with the mass ratio of 3:1;
s22, controlling the mass ratio of sodium alginate to stabilizer to water to be 5:3:22, adding water into sodium alginate, stirring at normal temperature until the sodium alginate is completely dissolved, adding stabilizer, continuously stirring until the sodium alginate is completely dissolved, and obtaining sodium alginate coating liquid, wherein the stabilizer comprises sophorolipid and polyethylene glycol 600 in a mass ratio of 5:1;
s23, adding nano graphene sheets (the thickness is 4-20nm, the diameter is 5-10 mu m, the number of layers is <30, the density is 0.23g/cm 3) into a silane coupling agent hydrolysate, controlling the stirring rotation speed to 450r/min, stirring at 60 ℃ for 1h, adding a plant extract, controlling the ultrasonic temperature to 50 ℃, controlling the ultrasonic power to 340W, performing ultrasonic frequency to 50kHz, performing ultrasonic dispersion for 1h, finally adding a sodium alginate coating solution, continuously stirring and mixing for 2h, and drying and curing at 80 ℃ to obtain a functional filler, wherein the mass ratio of the nano graphene sheets, the silane coupling agent hydrolysate, the plant extract and the sodium alginate coating solution is 6:20:1:12;
S3, preparing modified plant-based fibers:
S31, adding pine pulp with the solid content of 50% into boiling slurry according to the mass ratio of 1:5, boiling for 2 hours, filtering, immersing filter residues into sodium hypochlorite solution with the mass concentration of 22%, stirring for 1 hour at the temperature of 60 ℃, filtering, washing the filter residues, and drying to obtain cellulose pulp, wherein the boiling slurry is prepared by mixing sodium hydroxide, sodium sulfite and water according to the mass ratio of 1:4:18;
S32, adding cellulose pulp into an N-methylmorpholine-N-oxide aqueous solution with the mass concentration of 65% according to the mass ratio of 1:8, and stirring at the temperature of 90 ℃ until the cellulose pulp is completely dissolved to obtain a cellulose solution;
S33, mixing 100 parts by weight of cellulose solution, 30 parts by weight of functional filler, 8 parts by weight of epoxidized soybean oil and 3 parts by weight of potassium stearate for 30 minutes at a rotating speed of 450r/min, spinning the blend solution at a temperature of 90 ℃ through a spinning machine, curing by taking an acetic acid aqueous solution with a mass concentration of 33% at a temperature of 25 ℃ as a curing solution, drafting by a drafting multiple of 3 times, washing with ethanol, and drying at a temperature of 40 ℃ to obtain the modified plant-based fiber with a fineness of 2.5 dtex.
To verify the overall properties of the modified plant-based fibers produced in examples 1-5 of the present application, applicants set contrast agents 1-5, specifically as follows:
Comparative example 1
The lavender and valerian modified plant-based fiber is prepared by the following preparation method:
s1, preparing a plant extract:
Collecting fresh lavender and valerian, cleaning, airing, crushing, sieving with a 80-mesh sieve, mixing the lavender powder and the valerian powder according to a mass ratio of 1:3 to obtain plant powder, and primarily extracting the plant powder by a steam distillation method for 4 hours to obtain a plant extract;
s2, preparing functional filler:
S21, controlling the mass ratio to be 1:20, adding a silane coupling agent into an ethanol water solution with the mass fraction of 65%, and carrying out hydrolysis reaction for 2 hours at the temperature of 50 ℃ to obtain a silane coupling agent hydrolysate, wherein the silane coupling agent comprises gamma-glycidol ether oxypropyl trimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane with the mass ratio of 1:3;
s22, controlling the mass ratio of sodium alginate to stabilizer to water to be 5:2:22, adding water into sodium alginate, stirring at normal temperature until the sodium alginate is completely dissolved, adding stabilizer, continuously stirring until the sodium alginate is completely dissolved, and obtaining sodium alginate coating liquid, wherein the stabilizer comprises sophorolipid and polyethylene glycol 200 in a mass ratio of 3:1;
S23, adding nano graphene sheets (the thickness is 4-20nm, the diameter is 5-10 mu m, the density is 0.23g/cm 3) into a silane coupling agent hydrolysate, controlling the stirring rotation speed to be 350r/min, stirring at 50 ℃ for 2 hours, adding a plant extract, controlling the ultrasonic temperature to be 50 ℃, the ultrasonic power to be 280W, the ultrasonic frequency to be 40kHz, performing ultrasonic dispersion treatment for 2 hours, finally adding a sodium alginate coating solution, continuously stirring and mixing for 2 hours, and drying and curing at the temperature of 80 ℃ to obtain a functional filler, wherein the mass ratio of the nano graphene sheets, the silane coupling agent hydrolysate, the plant extract and the sodium alginate coating solution is 4:18:1:10;
S3, preparing modified plant-based fibers:
s31, adding pine pulp with the solid content of 50% into boiling slurry according to the mass ratio of 1:4, boiling for 2 hours, filtering, immersing filter residues into sodium hypochlorite solution with the mass concentration of 22%, stirring for 1 hour at the temperature of 60 ℃, filtering, washing the filter residues, and drying to obtain cellulose pulp, wherein the boiling slurry is prepared by mixing sodium hydroxide, sodium sulfite and water according to the mass ratio of 1:3:18;
s32, adding cellulose pulp into an N-methylmorpholine-N-oxide aqueous solution with the mass concentration of 55% according to the mass ratio of 1:6, and stirring at the temperature of 100 ℃ until the cellulose pulp is completely dissolved to obtain a cellulose solution;
S33, mixing 80 parts by weight of cellulose solution, 20 parts by weight of functional filler, 3 parts by weight of epoxidized soybean oil and 1 part by weight of potassium stearate for 40min at a rotating speed of 350r/min, spinning the blend solution at a temperature of 70 ℃ through a spinning machine, curing by taking an acetic acid aqueous solution with a mass concentration of 38% at a temperature of 20 ℃ as a curing solution, drafting by a drafting multiple of 2, washing with ethanol, and drying at a temperature of 60 ℃ to obtain the modified plant-based fiber with a fineness of 2.2 dtex.
Comparative example 2
The lavender and valerian modified plant-based fiber is prepared by the following preparation method:
s1, preparing a plant extract:
Collecting fresh lavender and valerian, cleaning, airing, crushing, sieving with a 80-mesh sieve, mixing the lavender powder and the valerian powder according to a mass ratio of 1:3 to obtain plant powder, adding an ethanol water solution with a mass concentration of 55% into the plant powder, performing ultrasonic extraction, controlling the ultrasonic temperature to be 50 ℃, the ultrasonic power to be 280W, the ultrasonic frequency to be 40kHz, performing ultrasonic extraction for 4 hours, and filtering to remove filter residues to obtain a plant extract;
s2, preparing functional filler:
S21, controlling the mass ratio to be 1:20, adding a silane coupling agent into an ethanol water solution with the mass fraction of 65%, and carrying out hydrolysis reaction for 2 hours at the temperature of 50 ℃ to obtain a silane coupling agent hydrolysate, wherein the silane coupling agent comprises gamma-glycidol ether oxypropyl trimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane with the mass ratio of 1:3;
s22, controlling the mass ratio of sodium alginate to stabilizer to water to be 5:2:22, adding water into sodium alginate, stirring at normal temperature until the sodium alginate is completely dissolved, adding stabilizer, continuously stirring until the sodium alginate is completely dissolved, and obtaining sodium alginate coating liquid, wherein the stabilizer comprises sophorolipid and polyethylene glycol 200 in a mass ratio of 3:1;
S23, adding nano graphene sheets (the thickness is 4-20nm, the diameter is 5-10 mu m, the density is 0.23g/cm 3) into a silane coupling agent hydrolysate, controlling the stirring rotation speed to be 350r/min, stirring at 50 ℃ for 2 hours, adding a plant extract, controlling the ultrasonic temperature to be 50 ℃, the ultrasonic power to be 280W, the ultrasonic frequency to be 40kHz, performing ultrasonic dispersion treatment for 2 hours, finally adding a sodium alginate coating solution, continuously stirring and mixing for 2 hours, and drying and curing at the temperature of 80 ℃ to obtain a functional filler, wherein the mass ratio of the nano graphene sheets, the silane coupling agent hydrolysate, the plant extract and the sodium alginate coating solution is 4:18:1:10;
S3, preparing modified plant-based fibers:
s31, adding pine pulp with the solid content of 50% into boiling slurry according to the mass ratio of 1:4, boiling for 2 hours, filtering, immersing filter residues into sodium hypochlorite solution with the mass concentration of 22%, stirring for 1 hour at the temperature of 60 ℃, filtering, washing the filter residues, and drying to obtain cellulose pulp, wherein the boiling slurry is prepared by mixing sodium hydroxide, sodium sulfite and water according to the mass ratio of 1:3:18;
s32, adding cellulose pulp into an N-methylmorpholine-N-oxide aqueous solution with the mass concentration of 55% according to the mass ratio of 1:6, and stirring at the temperature of 100 ℃ until the cellulose pulp is completely dissolved to obtain a cellulose solution;
S33, mixing 80 parts by weight of cellulose solution, 20 parts by weight of functional filler, 3 parts by weight of epoxidized soybean oil and 1 part by weight of potassium stearate for 40min at a rotating speed of 350r/min, spinning the blend solution at a temperature of 70 ℃ through a spinning machine, curing by taking an acetic acid aqueous solution with a mass concentration of 38% at a temperature of 20 ℃ as a curing solution, drafting by a drafting multiple of 2, washing with ethanol, and drying at a temperature of 60 ℃ to obtain the modified plant-based fiber with a fineness of 2.2 dtex.
Comparative example 3
The lavender and valerian modified plant-based fiber is prepared by the following preparation method:
s1, preparing a plant extract:
collecting fresh lavender and valerian, cleaning, airing, crushing, sieving with a 80-mesh sieve, mixing the lavender powder and the valerian powder according to a mass ratio of 1:3 to obtain plant powder, primarily extracting the plant powder by a steam distillation method for 2 hours to collect an extract I, then adding an ethanol water solution with a mass concentration of 55% into the plant powder according to a mass ratio of 1:8, performing ultrasonic extraction, controlling the ultrasonic temperature to be 50 ℃, the ultrasonic power to be 280W, performing ultrasonic extraction for 2 hours at an ultrasonic frequency of 40kHz, filtering to remove filter residues to obtain an extract II, and combining the extract I and the extract II to obtain a plant extract;
s2, preparing functional filler:
S21, controlling the mass ratio to be 1:20, adding a silane coupling agent into an ethanol water solution with the mass fraction of 65%, and carrying out hydrolysis reaction for 2 hours at the temperature of 50 ℃ to obtain a silane coupling agent hydrolysate, wherein the silane coupling agent comprises gamma-glycidol ether oxypropyl trimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane with the mass ratio of 1:3;
S22, controlling the mass ratio of sodium alginate to sophorolipid to water to be 5:2:22, adding water into sodium alginate, stirring at normal temperature until the sodium alginate is completely dissolved, adding sophorolipid, and continuously stirring until the sodium alginate is completely dissolved to obtain a sodium alginate coating liquid;
S23, adding nano graphene sheets (the thickness is 4-20nm, the diameter is 5-10 mu m, the density is 0.23g/cm 3) into a silane coupling agent hydrolysate, controlling the stirring rotation speed to be 350r/min, stirring at 50 ℃ for 2 hours, adding a plant extract, controlling the ultrasonic temperature to be 50 ℃, the ultrasonic power to be 280W, the ultrasonic frequency to be 40kHz, performing ultrasonic dispersion treatment for 2 hours, finally adding a sodium alginate coating solution, continuously stirring and mixing for 2 hours, and drying and curing at the temperature of 80 ℃ to obtain a functional filler, wherein the mass ratio of the nano graphene sheets, the silane coupling agent hydrolysate, the plant extract and the sodium alginate coating solution is 4:18:1:10;
S3, preparing modified plant-based fibers:
s31, adding pine pulp with the solid content of 50% into boiling slurry according to the mass ratio of 1:4, boiling for 2 hours, filtering, immersing filter residues into sodium hypochlorite solution with the mass concentration of 22%, stirring for 1 hour at the temperature of 60 ℃, filtering, washing the filter residues, and drying to obtain cellulose pulp, wherein the boiling slurry is prepared by mixing sodium hydroxide, sodium sulfite and water according to the mass ratio of 1:3:18;
s32, adding cellulose pulp into an N-methylmorpholine-N-oxide aqueous solution with the mass concentration of 55% according to the mass ratio of 1:6, and stirring at the temperature of 100 ℃ until the cellulose pulp is completely dissolved to obtain a cellulose solution;
S33, mixing 80 parts by weight of cellulose solution, 20 parts by weight of functional filler, 3 parts by weight of epoxidized soybean oil and 1 part by weight of potassium stearate for 40min at a rotating speed of 350r/min, spinning the blend solution at a temperature of 70 ℃ through a spinning machine, curing by taking an acetic acid aqueous solution with a mass concentration of 38% at a temperature of 20 ℃ as a curing solution, drafting by a drafting multiple of 2, washing with ethanol, and drying at a temperature of 60 ℃ to obtain the modified plant-based fiber with a fineness of 2.2 dtex.
Comparative example 4
The lavender and valerian modified plant-based fiber is prepared by the following preparation method:
s1, preparing a plant extract:
collecting fresh lavender and valerian, cleaning, airing, crushing, sieving with a 80-mesh sieve, mixing the lavender powder and the valerian powder according to a mass ratio of 1:3 to obtain plant powder, primarily extracting the plant powder by a steam distillation method for 2 hours to collect an extract I, then adding an ethanol water solution with a mass concentration of 55% into the plant powder according to a mass ratio of 1:8, performing ultrasonic extraction, controlling the ultrasonic temperature to be 50 ℃, the ultrasonic power to be 280W, performing ultrasonic extraction for 2 hours at an ultrasonic frequency of 40kHz, filtering to remove filter residues to obtain an extract II, and combining the extract I and the extract II to obtain a plant extract;
s2, preparing functional filler:
S21, controlling the mass ratio to be 1:20, adding a silane coupling agent into an ethanol water solution with the mass fraction of 65%, and carrying out hydrolysis reaction for 2 hours at the temperature of 50 ℃ to obtain a silane coupling agent hydrolysate, wherein the silane coupling agent comprises gamma-glycidol ether oxypropyl trimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane with the mass ratio of 1:3;
S22, controlling the mass ratio of sodium alginate to polyethylene glycol 200 to water to be 5:2:22, adding water into sodium alginate, stirring at normal temperature until the sodium alginate is completely dissolved, adding polyethylene glycol 200, and continuously stirring until the sodium alginate is completely dissolved to obtain sodium alginate coating liquid;
S23, adding nano graphene sheets (the thickness is 4-20nm, the diameter is 5-10 mu m, the density is 0.23g/cm 3) into a silane coupling agent hydrolysate, controlling the stirring rotation speed to be 350r/min, stirring at 50 ℃ for 2 hours, adding a plant extract, controlling the ultrasonic temperature to be 50 ℃, the ultrasonic power to be 280W, the ultrasonic frequency to be 40kHz, performing ultrasonic dispersion treatment for 2 hours, finally adding a sodium alginate coating solution, continuously stirring and mixing for 2 hours, and drying and curing at the temperature of 80 ℃ to obtain a functional filler, wherein the mass ratio of the nano graphene sheets, the silane coupling agent hydrolysate, the plant extract and the sodium alginate coating solution is 4:18:1:10;
S3, preparing modified plant-based fibers:
s31, adding pine pulp with the solid content of 50% into boiling slurry according to the mass ratio of 1:4, boiling for 2 hours, filtering, immersing filter residues into sodium hypochlorite solution with the mass concentration of 22%, stirring for 1 hour at the temperature of 60 ℃, filtering, washing the filter residues, and drying to obtain cellulose pulp, wherein the boiling slurry is prepared by mixing sodium hydroxide, sodium sulfite and water according to the mass ratio of 1:3:18;
s32, adding cellulose pulp into an N-methylmorpholine-N-oxide aqueous solution with the mass concentration of 55% according to the mass ratio of 1:6, and stirring at the temperature of 100 ℃ until the cellulose pulp is completely dissolved to obtain a cellulose solution;
S33, mixing 80 parts by weight of cellulose solution, 20 parts by weight of functional filler, 3 parts by weight of epoxidized soybean oil and 1 part by weight of potassium stearate for 40min at a rotating speed of 350r/min, spinning the blend solution at a temperature of 70 ℃ through a spinning machine, curing by taking an acetic acid aqueous solution with a mass concentration of 38% at a temperature of 20 ℃ as a curing solution, drafting by a drafting multiple of 2, washing with ethanol, and drying at a temperature of 60 ℃ to obtain the modified plant-based fiber with a fineness of 2.2 dtex.
Comparative example 5
The lavender and valerian modified plant-based fiber is prepared by the following preparation method:
s1, preparing a plant extract:
collecting fresh lavender and valerian, cleaning, airing, crushing, sieving with a 80-mesh sieve, mixing the lavender powder and the valerian powder according to a mass ratio of 1:3 to obtain plant powder, primarily extracting the plant powder by a steam distillation method for 2 hours to collect an extract I, then adding an ethanol water solution with a mass concentration of 55% into the plant powder according to a mass ratio of 1:8, performing ultrasonic extraction, controlling the ultrasonic temperature to be 50 ℃, the ultrasonic power to be 280W, performing ultrasonic extraction for 2 hours at an ultrasonic frequency of 40kHz, filtering to remove filter residues to obtain an extract II, and combining the extract I and the extract II to obtain a plant extract;
s2, preparing functional filler:
S21, controlling the mass ratio to be 1:20, adding a silane coupling agent into an ethanol water solution with the mass fraction of 65%, and carrying out hydrolysis reaction for 2 hours at the temperature of 50 ℃ to obtain a silane coupling agent hydrolysate, wherein the silane coupling agent comprises gamma-glycidol ether oxypropyl trimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane with the mass ratio of 1:3;
s22, controlling the mass ratio of sodium alginate to stabilizer to water to be 5:2:22, adding water into sodium alginate, stirring at normal temperature until the sodium alginate is completely dissolved, adding stabilizer, continuously stirring until the sodium alginate is completely dissolved, and obtaining sodium alginate coating liquid, wherein the stabilizer comprises sophorolipid and polyethylene glycol 200 in a mass ratio of 3:1;
S23, adding nano graphene sheets (the thickness is 4-20nm, the diameter is 5-10 mu m, the density is 0.23g/cm 3) into a silane coupling agent hydrolysate, controlling the stirring rotation speed to be 350r/min, stirring at 50 ℃ for 2 hours, controlling the ultrasonic temperature to be 50 ℃, the ultrasonic power to be 280W, the ultrasonic frequency to be 40kHz, performing ultrasonic dispersion treatment for 2 hours, finally adding a sodium alginate coating liquid, continuously stirring and mixing for 2 hours, and drying and curing at the temperature of 80 ℃ to obtain a functional filler, wherein the mass ratio of the nano graphene sheets, the silane coupling agent hydrolysate and the sodium alginate coating liquid is 2:9:5;
S3, preparing modified plant-based fibers:
s31, adding pine pulp with the solid content of 50% into boiling slurry according to the mass ratio of 1:4, boiling for 2 hours, filtering, immersing filter residues into sodium hypochlorite solution with the mass concentration of 22%, stirring for 1 hour at the temperature of 60 ℃, filtering, washing the filter residues, and drying to obtain cellulose pulp, wherein the boiling slurry is prepared by mixing sodium hydroxide, sodium sulfite and water according to the mass ratio of 1:3:18;
s32, adding cellulose pulp into an N-methylmorpholine-N-oxide aqueous solution with the mass concentration of 55% according to the mass ratio of 1:6, and stirring at the temperature of 100 ℃ until the cellulose pulp is completely dissolved to obtain a cellulose solution;
S33, stirring and mixing 80 parts by weight of cellulose solution, 20 parts by weight of functional filler, 3 parts by weight of epoxidized soybean oil and 1 part by weight of potassium stearate at a rotating speed of 350r/min for 40min, spinning the blend solution at a temperature of 70 ℃ through a spinning machine, curing by taking an acetic acid aqueous solution with a mass concentration of 38% at a temperature of 20 ℃ as a curing solution, drafting by a drafting multiple of 2, washing with ethanol, and drying at a temperature of 60 ℃ to obtain a plant-based fiber with a fineness of 2.2 dtex;
S34, controlling the mass ratio to be 1:18, adding the plant extract into the hydrolysate of the silane coupling agent, controlling the ultrasonic temperature to be 50 ℃ at the temperature of 45 ℃, controlling the ultrasonic power to be 280W, controlling the ultrasonic frequency to be 40kHz, performing ultrasonic dispersion treatment for 2 hours, adding the plant-based fiber into the solution containing the plant extract, soaking for 4 hours, taking out, and airing to obtain the modified plant-based fiber.
Performance testing
The modified base fibers prepared in examples 1 to 5 of the present application and comparative examples 1 to 5 were each tested for their combination properties.
Breaking strength and breaking elongation are tested according to the specification of test standard GB/T14344-2022;
the hygroscopicity is that 10g of each sample to be measured is respectively taken and placed in a drying oven to be dried to constant weight at 80 ℃, the weight of each sample after drying is recorded and marked as W 0, each sample after drying is respectively placed in an environment with the temperature of 37 ℃ and the relative humidity of 90% for 8 hours, the weight of each sample after moisture absorption is measured and marked as W 1, and the moisture absorption rate (%) = (W 1-W0)/W0 multiplied by 100;
The air permeability is that each sample to be tested is hot rolled and reinforced after being opened, carded, laid and meshed to prepare a non-woven fabric sample with the gram weight of 40g/m 2 and the thickness of 0.5mm, the non-woven fabric sample is tested according to the specification of the test standard GB/T5453-1997, the measurement is repeated for 10 times on different parts of each non-woven fabric sample, and the average value is calculated as the final air permeability of the test sample;
Antibacterial performance, namely testing staphylococcus aureus according to the specification of a test standard GB/T20944.3-2008;
The fragrance release period is to take 10g of each sample to be tested and put the sample into a sealing bag, seal the bag for 1h at the temperature of 60 ℃ and smell the fragrance, take the sample as a cycle, test the fragrance completely until the fragrance is lost, and record the cycle test times when the fragrance is lost;
The sleep-aiding effect is that each sample to be tested is filled into a pillow to be tested, the average falling time is more than 30min within nearly two months, the average total sleeping time is less than 7h, the average deep sleeping time is less than 0.8h, 22 volunteers with the age of 35-55 years are randomly divided into 11 groups, each pillow to be tested is respectively used, sleep monitoring is carried out on the volunteers by using a sleep monitor, the monitoring time is 8h, the monitoring index is falling time and deep sleeping time, the monitoring period is 30 days, after the numerical value with obvious deviation in the monitored data is removed, the rest data are averaged, and the average falling time t 1 and the average deep sleeping time t 2 are obtained.
The specific performance test results are shown in table 1 below:
The results shown in the table 1 show that the comprehensive performance of the modified base fibers prepared in the examples 1-5 is obviously better than that of the modified base fibers prepared in the comparative examples 1-5, namely, the prepared modified base fibers can obviously improve the health care performance and antibacterial and anti-inflammatory performance of the fibers and increase the moisture absorption and air permeability of the fibers while ensuring the excellent mechanical performance and the heat stability performance within the limit technical scheme of the application.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
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