CN113981555A - Aromatic regenerated cellulose fiber, fabric and preparation method - Google Patents
Aromatic regenerated cellulose fiber, fabric and preparation method Download PDFInfo
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- CN113981555A CN113981555A CN202111484352.5A CN202111484352A CN113981555A CN 113981555 A CN113981555 A CN 113981555A CN 202111484352 A CN202111484352 A CN 202111484352A CN 113981555 A CN113981555 A CN 113981555A
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- China
- Prior art keywords
- essential oil
- cellulose fiber
- solution
- regenerated cellulose
- aromatic
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- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 103
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title description 4
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- 229920000297 Rayon Polymers 0.000 claims abstract description 19
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- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 38
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Images
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
Abstract
The invention provides an aromatic regenerated cellulose fiber, fabric and a preparation method, and particularly relates to the technical field of spinning. The preparation method of the aromatic regenerated cellulose fiber comprises the following steps: preparing plant essential oil microcapsules; adding the plant essential oil microcapsule, chitosan and a viscose crosslinking agent into a cellulose fiber spinning solution according to a certain proportion, and uniformly stirring to obtain a mixed solution; and spinning the mixed solution to obtain the aromatic regenerated cellulose fiber. The plant essential oil microcapsule is a double-layer microcapsule, so that the slow release property and stability of the microcapsule can be improved, the efficacy time of the microcapsule can be prolonged, and the regenerated cellulose fiber can obtain a lasting aromatic function; the fabric prepared from the aromatic regenerated cellulose fibers not only maintains the advantages of the regenerated fiber fibers, but also has the effects of soothing the nerves, protecting health, resisting bacteria and the like by using the plant essential oil.
Description
Technical Field
The invention relates to the technical field of textiles, and particularly relates to an aromatic regenerated cellulose fiber, fabric and a preparation method.
Background
Regenerated cellulose fibers are popular materials for textile materials, and are cellulose fibers obtained by recovering natural cellulose fiber clothing products such as cotton, hemp, bamboo, and rayon, waste materials thereof, or cellulose components extracted from bark, crops, and plants, and processing the cellulose components. Because of 100 percent of pure natural materials, the fiber is naturally biodegradable, has no additive, heavy metal or harmful chemical substances, is compatible and nonirritating to skin, and is environment-friendly green fiber with excellent performance. The regenerated cellulose fiber fabric is known as breathable fabric, has soft hand feeling, smoothness, coolness and uneasy static electricity, and has the advantages of softness of cotton, luster of silk and smoothness of hemp; comfortable and close fitting, air permeability and moisture absorption, and good elasticity; the cotton-padded clothes do not feel sultry when worn in summer, and the air permeability is superior to that of pure cotton fabric, so that the cotton-padded clothes are ideal close-fitting fabrics and health-care clothing products. However, with the rapid development of economy and the acceleration of life rhythm, people are under greater pressure, the sleep quality is reduced due to long-term emotional stress and excessive psychological load, and a series of psychological and physiological diseases are caused by sleep problems. Therefore, the home textile with the sleep health care function is favored by more and more people, and the single regenerated cellulose fiber fabric meets the requirements of the home textile.
The plant essential oil has the effects of soothing nerves, protecting health, resisting bacteria and the like, so the plant essential oil is widely applied to various industries such as food, daily chemicals, medicines, textiles and the like. However, the essential oil has the characteristics of unsaturated bonds, easy volatilization and the like, has short fragrance retention period, causes the defects of short fragrance retention time, uncontrollable release and the like, is inconvenient to store, transport, diversify in medicament dosage forms and the like, is easy to deteriorate under the influence of factors such as light, heat, air and the like, and limits the action effect and the application range of the essential oil. Especially in the field of textiles, the aromatic fabric prepared by processing the essential oil needs to be washed and dried in the using process, and in the period, the loss of fragrance is large due to the action of external force, so that the textile cannot play the expected effect after being used for a long time, and the requirements of people cannot be met. Therefore, there is a need to develop a fabric capable of maintaining the fragrance function for a long time.
Disclosure of Invention
In view of the defects of the prior art, the invention provides an aromatic regenerated cellulose fiber, fabric and a preparation method thereof, so as to solve the problem that the regenerated cellulose fiber fabric cannot meet the sleep health care requirement.
To achieve the above and other related objects, the present invention provides a method for preparing aromatic regenerated cellulose fiber, which comprises at least the following steps: preparing plant essential oil microcapsules; adding the plant essential oil microcapsule, chitosan and a viscose crosslinking agent into a cellulose fiber spinning solution according to a certain proportion, and uniformly stirring to obtain a mixed spinning solution; spinning the mixed solution to obtain aromatic regenerated cellulose fibers; the plant essential oil microcapsule comprises, by mass, 8-20 parts of plant essential oil microcapsules, 5-10 parts of chitosan, 2-10 parts of a viscose crosslinking agent and 1000 parts of a cellulose fiber spinning solution, wherein the cellulose fiber spinning solution contains 8-15 wt% of cellulose.
In one example of the present invention, the preparation of the plant essential oil microcapsule comprises the following steps: firstly, preparing a core material solution by using plant essential oil; preparing a wall material solution by using cyclodextrin; adding the core material solution into the wall material solution, homogenizing and emulsifying to realize primary cyclodextrin coating of the plant essential oil; and then the plant essential oil is embedded for the second time by utilizing chitosan/sodium alginate to obtain the double-layer microcapsule.
In one example of the invention, when preparing the core material solution, the plant essential oil and the absolute ethyl alcohol are uniformly mixed according to the mass ratio of 1 (2-5), lecithin is added into the mixed solution, and the mixed solution is heated to be completely dissolved, wherein the mass ratio of the plant essential oil to the lecithin is (1-5) to 2.
In one example of the invention, the plant essential oil comprises one or more of lavender essential oil, chamomile essential oil, vanilla essential oil, and valerian essential oil.
In an example of the present invention, when preparing a wall material solution, 60 to 80 parts by mass of cyclodextrin, 10 to 25 parts by mass of sodium starch octenyl succinate and 5 to 12 parts by mass of emulsification modified starch are added into water and stirred at 50 to 70 ℃ for 1 hour, 5 to 10 parts by mass of an emulsifier are added, and the mixture is mixed and stirred for 20 minutes, wherein the mass ratio of the total mass of the cyclodextrin, the sodium starch octenyl succinate and the emulsification modified starch to the water is 1: (4-10).
In one example of the invention, the cyclodextrin includes a mixture of one or more of alpha-cyclodextrin, beta-cyclodextrin, hydroxypropyl beta-cyclodextrin, hydroxymethyl beta-cyclodextrin, hydroxyethyl beta-cyclodextrin.
In one example of the present invention, the emulsifier includes a mixture of one or more of polyether modified silicone, polyether modified organofluorine, alkyl polyether, tween 40, tween 60, tween 80, sodium dodecylbenzenesulfonate, and sodium dodecylsulfate.
In one example of the present invention, the cyclodextrin primary entrapped plant essential oil comprises: adding the core material solution into the wall material solution, and stirring for 20-60 min at 40-60 ℃; and (3) homogenizing and emulsifying the mixed solution of the core material solution and the wall material solution by using a homogenizer to obtain a stable emulsifying system, and drying the stable emulsifying system to obtain the single-layer microcapsule.
In one example of the present invention, the homogenizing and emulsifying includes a first homogenizing and a second homogenizing, wherein the first homogenizing is performed at a rotation speed of 5000-20000 rpm for 5-20 min under a pressure of 100-500 bar; and the secondary homogenization is to add liquid paraffin into the emulsion obtained by the primary homogenization, and homogenize for 5-20 min again, wherein the addition amount of the liquid paraffin is 0.5-2% of the total mass of the emulsion.
In an example of the present invention, the secondary embedding includes: adding the single-layer microcapsule obtained by primary embedding into a sodium alginate solution, and uniformly stirring at 50-60 ℃ to obtain a mixed solution; adding chitosan and calcium chloride into the mixed solution, stirring uniformly, and carrying out ultrasonic treatment for 5 min; filtering and drying to obtain the double-layer microcapsule.
In one example of the invention, the sodium alginate solution comprises 3-8 wt% of sodium alginate, 2-4 wt% of polyethylene glycol and 1% of dibutyl tin dilaurate; the concentration of the chitosan in the mixed system is 2-3 wt% (the mass of the chitosan accounts for the total mass of the mixed system), and the concentration of the calcium chloride in the mixed system is 0.5-2 wt% (the mass of the calcium chloride accounts for the total mass of the mixed system).
In an example of the invention, the viscose cross-linking agent is prepared by diluting the cellulose fiber spinning solution to 5-6 wt% of methyl cellulose, adding 0.1-0.2 wt% of polyacrylamide and 0.1-0.2 wt% of hydrogen peroxide, and mixing and stirring uniformly.
In one example of the present invention, the cellulose fiber spinning solution is prepared from pulp with a polymerization degree of 500 to 800.
The invention also provides aromatic regenerated cellulose fiber which is prepared by the preparation method, and the aromatic regenerated cellulose fiber comprises the following raw materials in parts by weight: 8-20 parts of plant essential oil microcapsules, 5-10 parts of chitosan, 2-10 parts of viscose crosslinking agents and 1000 parts of cellulose fiber spinning solution; wherein the cellulose content in the cellulose fiber spinning solution is 8-15 wt%.
In an example of the present invention, the plant essential oil microcapsule includes a core material, a first wall material and a second wall material, the first wall material is coated on an outer side of the core material, the second wall material is coated on an outer side of the first wall material, the core material is plant essential oil, the first wall material is cyclodextrin, and the second wall material is chitosan/sodium alginate.
In a third aspect, the present invention provides an aromatic fabric woven from the aromatic regenerated cellulose fibers of the present invention.
The invention provides a preparation method of aromatic regenerated cellulose, which is characterized in that plant essential oil microcapsules are added into cellulose spinning solution according to a certain proportion, and the aromatic regenerated cellulose fiber is obtained through dry spinning or wet spinning. The plant essential oil microcapsule is a double-layer microcapsule obtained by coating essential oil molecules in a cyclodextrin cavity by utilizing the special cavity structure and the characteristics of internal hydrophobicity and external hydrophilicity of cyclodextrin to form a microcapsule with a molecular level and then carrying out secondary embedding on plant essential oil by utilizing chitosan/sodium alginate, so that the slow release property and the stability of the microcapsule are improved, the effect action time of the microcapsule is prolonged, and the aromatic regenerated cellulose fiber has a lasting aromatic function; the fabric prepared from the aromatic regenerated cellulose fibers not only maintains the advantages of the regenerated fiber fibers, but also has the effects of soothing the nerves, protecting health, resisting bacteria and the like by using the plant essential oil. The preparation method of the invention has the advantages of low cost, simple process, no toxicity and no harm.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of a method of making aromatic regenerated cellulose fibers of the present invention;
FIG. 2 is a flow chart of the preparation of plant essential oil microcapsules in FIG. 1;
fig. 3 is a flow chart of the preparation of the cellulose fiber spinning solution.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It is to be noted that the features in the following embodiments and examples may be combined with each other without conflict. It is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention. Test methods in which specific conditions are not specified in the following examples are generally carried out under conventional conditions or under conditions recommended by the respective manufacturers.
It should be understood that the terms "upper", "lower", "left", "right", "middle" and "one" used herein are for clarity of description only, and are not intended to limit the scope of the invention, and that changes or modifications in the relative relationship may be made without substantial technical changes and modifications.
Referring to fig. 1 and 2, the present invention provides an aromatic regenerated cellulose fiber, a fabric and a preparation method thereof, so as to obtain a regenerated cellulose fiber fabric with a health care function.
Referring to fig. 1, the preparation method of the aromatic regenerated cellulose fiber of the present invention at least includes the following steps:
s1, preparing plant essential oil microcapsules;
s2, adding the plant essential oil microcapsules, chitosan and a viscose cross-linking agent into the cellulose fiber spinning solution according to a certain proportion, and uniformly mixing and stirring to obtain a mixed solution;
and S3, spinning the mixed solution to obtain the aromatic regenerated cellulose fiber.
The plant essential oil microcapsule in step S1 is a double-layer microcapsule, which includes a core material, a first wall material and a second wall material, the first wall material is wrapped on the outer side of the core material, the second wall material is wrapped on the outer side of the first wall material, the core material is plant essential oil, such as rose essential oil, honeysuckle essential oil, rosemary essential oil, mint essential oil, pine needle essential oil, folium artemisiae argyi essential oil, and the like, the type of the plant essential oil is not limited herein, and the plant essential oil can be specifically selected according to the efficacy of the essential oil. In the embodiment, lavender essential oil, chamomile essential oil, vanilla essential oil, valerian essential oil and the like with a nerve soothing effect are selected, the first wall material is cyclodextrin, and the second wall material is chitosan/sodium alginate.
In the step S2, the plant essential oil microcapsule is 8-20 parts by mass, the chitosan is 5-10 parts by mass, the viscose crosslinking agent is 2-10 parts by mass, the cellulose fiber spinning solution is 1000 parts by mass, and the content of alpha fibers in the cellulose fiber spinning solution is 8-15 wt%.
The spinning in step S3 may be dry spinning or wet spinning.
Referring to fig. 1 and 2, the step S1 of preparing plant essential oil microcapsules at least comprises the following steps:
s11, preparing a core material solution by using plant essential oil;
s12, preparing a wall material solution by using cyclodextrin;
s13, adding the core material solution into the wall material solution, homogenizing and emulsifying to realize primary embedding of plant essential oil by cyclodextrin;
s14, carrying out secondary embedding on the plant essential oil by utilizing the chitosan/sodium alginate to obtain the double-layer microcapsule.
Referring to fig. 2, in step S11, the core solution is prepared by mixing the plant essential oil and absolute ethanol in a ratio of 1: and (2) uniformly mixing and stirring the mixture according to the mass ratio of (2-5), adding lecithin into the solution, heating and stirring the mixture to completely dissolve the lecithin into the solution to obtain a core material solution, wherein the mass ratio of the plant essential oil to the lecithin is (1-5) to 2. The plant essential oil can be selected from one or more of lavender essential oil, chamomile essential oil, vanilla essential oil and valerian essential oil, and of course, other types of plant essential oils can be selected and can be selected according to the specific efficacy of the essential oil. Lecithin is a natural antidote, and a certain amount of lecithin is added into plant essential oil to decompose toxin in vivo and provide sufficient nutrients such as water, oxygen and the like for skin by increasing heme, so that the skin becomes smooth and soft. In some embodiments, the mass ratio of the plant essential oil to the absolute ethyl alcohol can be selected to be 1:2, 1:3, 1:5, etc., and the mass ratio of the plant essential oil to the lecithin can be selected to be 1:2, 3:2, 5:2, etc., and both endpoints and middle values in the above ratio range can be selected.
Referring to fig. 2, when preparing the wall material solution in step S12, the prepared wall material is added into water and stirred at 50-70 ℃ for 1 hour, and then the emulsifier is added to mix and stir for 20min for emulsification, wherein the mass ratio of the wall material to the water is 1: (4-10), for example, 1:4, 1:6, 1:8, 1:10, etc. The wall material comprises 60-80 parts by mass of cyclodextrin, 10-25 parts by mass of sodium starch octenylsuccinate and 5-12 parts by mass of emulsified modified starch, wherein the cyclodextrin can be selected from one or a mixture of more of alpha-cyclodextrin, beta-cyclodextrin, hydroxypropyl beta-cyclodextrin, hydroxymethyl beta-cyclodextrin and hydroxyethyl beta-cyclodextrin. The cyclodextrin has the characteristics of special cavity structure, internal hydrophobicity and external hydrophilicity, and essential oil molecules enter the cyclodextrin cavity through intermolecular acting forces such as hydrophobic action, van der Waals force, hydrogen bonds and the like to form a microcapsule at a molecular level.
The emulsifier is 5-10 parts by weight, and can be selected from one or a mixture of polyether modified organic silicon, polyether modified organic fluorine, alkyl polyether, tween 40, tween 60, tween 80, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate. The emulsifier can reduce the interfacial tension in the mixing system and prevent the mutual coagulation and aggregation of the liquid drops to form uniform emulsion.
Referring to fig. 2, the step S13 of primary embedding specifically includes: and (3) adding the core material solution prepared in the step (S11) into the wall material solution prepared in the step (S12), uniformly stirring at 40-60 ℃, for example, stirring for 20-60 min, homogenizing the uniformly stirred mixed solution by using a homogenizer to obtain a stable emulsifying system, and drying the emulsifying system to obtain the single-layer microcapsule. Wherein the mass ratio of the core material solution to the wall material solution is 1 (0.5-1.5), for example, 1:0.5, 1:1 or 1: 1.5.
In one embodiment, the homogenizing treatment comprises primary homogenizing and secondary homogenizing, namely, the uniformly stirred mixed solution is placed in a homogenizing bag, and is homogenized and emulsified for 5-20 min at the rotating speed of 5000-20000 rpm under the pressure of 100-500 bar; and then adding liquid paraffin into the emulsion system, and carrying out secondary homogenization for 5-20 min under the same pressure and rotation speed, wherein the addition amount of the liquid paraffin is 0.5-2% of the total mass of the emulsion during the secondary homogenization. Because the cyclodextrin is in a porous structure, the plant essential oil is wrapped by the cyclodextrin, the plant essential oil can volatilize from the gaps of the cyclodextrin, the gaps of the cyclodextrin can be wrapped by the liquid paraffin, and the loss of the essential oil in the subsequent heating process is reduced.
Referring to fig. 2, the step S14 of secondary embedding specifically includes: slowly adding the single-layer microcapsule obtained in the step S3 into a sodium alginate solution, and uniformly stirring at 50-60 ℃ to obtain a mixed solution; slowly adding chitosan and calcium chloride into the mixed solution, mixing and stirring uniformly, performing ultrasonic treatment for 5min, filtering and drying, and wrapping chitosan/sodium alginate on the outer side of the cyclodextrin to form a double-layer microcapsule. The mass of the single-layer microcapsule is 15-30% of that of a sodium alginate solution, the sodium alginate solution comprises 3-8% of sodium alginate, 2-4% of polyethylene glycol and 1% of dibutyltin dilaurate in mass fraction, the concentration of chitosan in a mixed system is 2-3 wt%, and the concentration of calcium chloride in the mixed system is 0.5-2 wt%.
The formation mechanism of the chitosan/sodium alginate biological capsule is as follows: the chitosan is a high molecular substance formed by connecting 2-amino-glucose through beta-1, 4 glycosidic bonds, a large amount of primary amino groups exist in molecules, the chitosan is positively charged, the sodium alginate is formed by polymerizing sodium salt (M) of d-type mannuronic acid with a beta-1, 4 structure and L-type guluronic acid (G) with an alpha-1, 4 structure, the molecules are provided with a large amount of carboxyl groups and negatively charged, when the chitosan, the sodium alginate and calcium chloride coexist, the chitosan and the sodium alginate are attracted by the positive and negative charges to form a polyelectrolyte membrane, and the sodium alginate and the Ca are adsorbed by the positive and negative charges2+The complex forms a cured film, and the mechanism diagram is as follows:
directly pluck into sodium alginate solution with chitosan and calcium chloride, at first chitosan and sodium alginate form the complex layer, along with sodium alginate and chitosan further reaction, the complex layer thickens, and chitosan deposits at the inner membrane of complex layer simultaneously, and along with the thickening of complex layer, the liquid drop further contracts, and the Ca in the membrane is further+Exuding under the action of concentration difference and mechanical force, reacting with sodium alginate, forming calcium alginate coacervate outside the complex layer, and finally forming a three-layer film containing calcium alginate coacervate, chitosan/sodium alginate complex layer and chitosan precipitate layer.
Referring to fig. 1, in step S2, the cellulose fiber spinning solution is prepared by using pulp with a polymerization degree of 500-800 as a raw material, and sequentially performing impregnation, squeezing, crushing, aging, yellowing, continuous dissolution, filtration, and defoaming treatments. Pulp undergoes two chemical actions during the preparation process: the pulp reacts with alkali to generate alkali cellulose, and then the alkali cellulose reacts with sulfur dioxide to generate fiber xanthate, and the specific process flow is shown in figure 3. The production process of the cellulose fiber spinning solution is the prior art, and the parts which are not described in detail can refer to the prior art.
The viscose cross-linking agent is obtained by diluting a certain amount of cellulose fiber spinning solution with water until the content of methyl fibers is 5-6 wt%, adding polyacrylamide and 10% hydrogen peroxide, and mixing and stirring uniformly, wherein the addition amount of polyacrylamide is 0.1-0.2 wt% of the mass of the cellulose fiber spinning solution, and the addition amount of hydrogen peroxide is 0.1-0.2 wt% of the mass of the cellulose fiber spinning solution.
Referring to fig. 1, the spinning in step S3 may be dry spinning or wet spinning, for example, when wet spinning is adopted, the mixed solution of the plant essential oil microcapsules prepared in step S2 and the cellulose spinning solution is fed into a wet spinning machine to be spun according to a spinning process, and the specific process of wet spinning may refer to the existing process. Wherein the specification of the spinneret is 21000 holes multiplied by 0.06mm, the spinning speed is 55m/min, the components of the coagulating bath comprise 115g/L of sulfuric acid, 325g/L of sodium sulfate and 11.5g/L of zinc sulfate, the temperature of the coagulating bath is 52 ℃, and the temperature of the plasticizing bath is 95 ℃.
The aromatic regenerated cellulose fiber prepared by the invention can be used for obtaining the aromatic fabric through a textile process, wherein the textile process comprises but is not limited to spinning, knitting, tatting, non-weaving and the like. The aromatic fabric prepared by the invention can still keep the aromatic function after hundreds of washing tests, and can be used for home textile products, clothes and the like.
The invention will now be described in more detail by means of several specific examples, the cellulose fiber dope used in the following examples having an alpha fiber content of 8.9% by weight, a viscosity of 59 seconds (drop ball test, i.e. the time required for a 2mm steel ball to fall 20cm from the viscose solution), a degree of ripeness (using NH at a concentration of 10%)4Cl solution assay) was 8.8 mL.
Example 1
This example of preparing aromatic regenerated cellulose fibers includes the following steps:
preparing plant essential oil microcapsules: firstly, uniformly mixing and stirring lavender essential oil and absolute ethyl alcohol in a mass ratio of 1:2, adding lecithin into the mixed solution, wherein the mass ratio of the plant essential oil to the lecithin is 1:2, and heating and stirring to completely dissolve the plant essential oil and the lecithin to obtain a core material solution; adding 70 parts by mass of beta-cyclodextrin, 20 parts by mass of sodium starch octenylsuccinate and 10 parts by mass of emulsified modified starch into water (the mass ratio of the total mass of the components to the water is 1:4), stirring for 1h at 60 ℃, adding 8 parts by mass of tween-80, and continuously stirring for 20min to obtain a wall material solution; mixing the core material solution and the wall material solution in a mass ratio of 1:1.5, and stirring at 50 ℃ for 40 min; homogenizing the mixed system of the core material and the pipe material for 20min at the rotating speed of 20000rpm under the pressure of 500bar by using a nano homogenizer, adding liquid paraffin accounting for 1 wt% of the mixed system, homogenizing for 20min to obtain a stable emulsifying system, and drying to obtain the cyclodextrin-coated single-layer microcapsule; adding the single-layer microcapsule into a sodium alginate solution (8 wt% of sodium alginate, 3 wt% of polyethylene glycol and 1 wt% of dibutyltin dilaurate), wherein the addition amount of the single-layer microcapsule is 30 wt% of the mass of the sodium alginate solution, and uniformly stirring at 50 ℃ to obtain a mixed solution; slowly adding chitosan and calcium chloride (the addition amount of chitosan is 3 wt% of the total system, and the addition amount of calcium chloride is 2 wt% of the total system), stirring and mixing uniformly, performing ultrasonic treatment for 5min, filtering, and drying to obtain the double-layer microcapsule.
Preparation of a viscose crosslinker: and (2) adding water into a certain amount of cellulose fiber spinning solution to dilute until the content of alpha fibers is 5-6 wt%, adding polyacrylamide and 10% hydrogen peroxide, and mixing and stirring uniformly, wherein the addition amount of polyacrylamide is 0.16 wt% of the mass of the cellulose fiber spinning solution, and the addition amount of hydrogen peroxide is 0.15 wt% of the mass of the cellulose fiber spinning solution.
Preparing aromatic regenerated cellulose fiber: adding 15 parts of plant essential oil microcapsules, 8 parts of chitosan and 5 parts of viscose crosslinking agent into 1000 parts of cellulose fiber spinning solution, uniformly stirring to obtain a mixed solution, and performing wet spinning on the mixed solution to obtain the aromatic regenerated cellulose fibers.
The aromatic regenerated cellulose fiber prepared in the embodiment is prepared into fabric, and the fabric is subjected to water washing test, so that the fabric can still keep faint scent after being washed for 200 times.
Example 2
This example of preparing aromatic regenerated cellulose fibers includes the following steps:
preparing plant essential oil microcapsules: firstly, uniformly mixing and stirring lavender essential oil and absolute ethyl alcohol in a mass ratio of 1:3, adding lecithin into the mixed solution, wherein the mass ratio of the plant essential oil to the lecithin is 3:2, and heating and stirring to completely dissolve the plant essential oil and the lecithin to obtain a core material solution; adding 80 parts by mass of beta-cyclodextrin, 10 parts by mass of sodium starch octenylsuccinate and 12 parts by mass of emulsified modified starch into water (the mass ratio of the total mass of the components to the water is 1:10), stirring for 1h at 70 ℃, adding 10 parts by mass of tween-40, and continuously stirring for 20min to obtain a wall material solution; mixing the core material solution and the wall material solution in a mass ratio of 1:1, and stirring at 50 ℃ for 40 min; homogenizing the mixed system of the core material and the pipe material for 20min at the rotation speed of 10000rpm under the pressure of 500bar by using a nano homogenizer, adding liquid paraffin accounting for 2 wt% of the mixed system, homogenizing for 20min to obtain a stable emulsifying system, and drying the stable emulsifying system to obtain the cyclodextrin-coated single-layer microcapsule; adding the single-layer microcapsule into a sodium alginate solution (5 wt% of sodium alginate, 2 wt% of polyethylene glycol and 1 wt% of dibutyltin dilaurate), wherein the addition amount of the single-layer microcapsule is 20 wt% of the mass of the sodium alginate solution, and uniformly stirring at 50 ℃ to obtain a mixed solution; slowly adding chitosan and calcium chloride (the addition amount of chitosan is 2 wt% of the total system, and the addition amount of calcium chloride is 1 wt% of the total system), stirring and mixing uniformly, performing ultrasonic treatment for 5min, filtering, and drying to obtain the double-layer microcapsule.
Preparation of a viscose crosslinker: and (2) adding water into a certain amount of cellulose fiber spinning solution to dilute until the content of alpha fibers is 5-6 wt%, adding polyacrylamide and 10% hydrogen peroxide, and mixing and stirring uniformly, wherein the addition amount of polyacrylamide is 0.12 wt% of the mass of the cellulose fiber spinning solution, and the addition amount of hydrogen peroxide is 0.18 wt% of the mass of the cellulose fiber spinning solution.
Preparing aromatic regenerated cellulose fiber: adding 20 parts of plant essential oil microcapsules, 5 parts of chitosan and 10 parts of viscose crosslinking agent into 1000 parts of cellulose fiber spinning solution, uniformly stirring to obtain a mixed solution, and performing wet spinning on the mixed solution to obtain the aromatic regenerated cellulose fibers.
The aromatic regenerated cellulose fiber prepared in the embodiment is prepared into fabric, and the fabric is subjected to water washing test, so that the fabric can still keep faint scent after being washed for 180 times.
Example 3
This example of preparing aromatic regenerated cellulose fibers includes the following steps:
preparing plant essential oil microcapsules: firstly, uniformly mixing and stirring lavender essential oil and absolute ethyl alcohol in a mass ratio of 1:5, adding lecithin into the mixed solution, wherein the mass ratio of the plant essential oil to the lecithin is 5:2, and heating and stirring to completely dissolve the plant essential oil and the lecithin to obtain a core material solution; adding 60 parts by mass of beta-cyclodextrin, 10 parts by mass of sodium starch octenylsuccinate and 12 parts by mass of emulsified modified starch into water (the mass ratio of the total mass of the components to the water is 1:7), stirring for 1h at 60 ℃, adding 8 parts by mass of tween-60, and continuously stirring for 20min to obtain a wall material solution; mixing the core material solution and the wall material solution in a mass ratio of 1:0.5, and stirring at 50 ℃ for 40 min; homogenizing the mixed system of the core material and the pipe material for 20min at the rotation speed of 20000rpm under the pressure of 500bar by using a nano homogenizer, adding liquid paraffin with the weight percent of 0.5 percent of the mixed system, homogenizing for 20min to obtain a stable emulsifying system, and drying the stable emulsifying system to obtain a cyclodextrin-coated single-layer microcapsule; adding the single-layer microcapsule into a sodium alginate solution (3 wt% of sodium alginate, 4 wt% of polyethylene glycol and 1 wt% of dibutyltin dilaurate), wherein the addition amount of the single-layer microcapsule is 15 wt% of the mass of the sodium alginate solution, and uniformly stirring at 50 ℃ to obtain a mixed solution; slowly adding chitosan and calcium chloride (the addition amount of chitosan is 2.5 wt% of the total system, and the addition amount of calcium chloride is 0.5 wt% of the total system), stirring and mixing uniformly, performing ultrasonic treatment for 5min, filtering, and drying to obtain the double-layer microcapsule.
Preparation of a viscose crosslinker: adding water into a certain amount of cellulose fiber spinning solution to dilute the cellulose fiber spinning solution until the content of alpha fibers is 5-6 wt%, adding polyacrylamide and 10% hydrogen peroxide, and uniformly mixing and stirring, wherein the addition amount of polyacrylamide is 0.1 wt% of the mass of the cellulose fiber spinning solution, and the addition amount of hydrogen peroxide is 0.2 wt% of the mass of the cellulose fiber spinning solution.
Preparing aromatic regenerated cellulose fiber: adding 8 parts of plant essential oil microcapsules, 10 parts of chitosan and 8 parts of viscose crosslinking agent into 1000 parts of cellulose fiber spinning solution, uniformly stirring to obtain a mixed solution, and performing wet spinning on the mixed solution to obtain the aromatic regenerated cellulose fibers.
The aromatic regenerated cellulose fiber prepared in the embodiment is prepared into fabric, and the fabric is subjected to water washing test, so that the fabric can still keep faint scent after being washed for 160 times.
Example 4
The difference of this example compared with example 1 is that lavender essential oil is replaced by chamomile essential oil, and other conditions are not changed. The aromatic regenerated cellulose fiber prepared in the embodiment is prepared into fabric, and the fabric is subjected to water washing test, so that the fabric can still keep faint scent after being washed for 190 times.
Example 5
The difference of this example compared with example 2 is that the lavender essential oil is replaced by the vanilla essential oil, and other conditions are not changed. The aromatic regenerated cellulose fiber prepared in the embodiment is prepared into fabric, and the fabric is subjected to water washing test, so that the fabric can still keep faint scent after being washed for 180 times.
Example 6
The difference between this example and example 3 is that the lavender essential oil is replaced by valerian essential oil, and other conditions are not changed. The aromatic regenerated cellulose fiber prepared in the embodiment is prepared into fabric, and the fabric is subjected to water washing test, so that the fabric can still keep faint scent after being washed for 160 times.
Comparative example 1
The difference between comparative example 1 and example 1 is that: the plant essential oil microcapsule is not subjected to homogenization treatment and secondary embedding in the preparation process. The aromatic regenerated cellulose fiber prepared in comparative example 1 was prepared into a fabric, and the fabric was subjected to a water washing test, and no significant fragrance was observed after 50 times of washing.
Indexes of the plant essential oil microcapsules prepared in examples 1 to 6 and comparative example 1 were measured, and the results are shown in table 1:
table 1: results of examination of the products obtained in examples 1 to 6 and comparative example 1
The detection results of the examples 1 to 6 and the comparative example 1 show that the embedding rate of the plant essential oil microcapsule is 60 to 80 percent, the particle size of the microcapsule is less than 50 mu m, and most of the particle sizes are concentrated in 1 to 10 mu m. Compared with the particle size distribution of the comparative example 1 which is 10-200 mu m, the particle size distribution of the preparation method is smaller and the embedding rate is better in the preparation method of the invention compared with the comparative example 1.
The retention of the products obtained in examples 1 to 6 and comparative example 1 was examined to evaluate the stability effect:
the products of examples 1 to 6 and comparative example 1 were equally divided into 4 groups of test samples, which were respectively left at normal temperature for 3 months and at high temperature (100 ℃, 130 ℃, 160 ℃) for 72 hours, and the samples were periodically withdrawn, and the content of essential oil in each sample was measured by hplc to examine the retention rates at normal temperature and high temperature, and the results are shown in tables 2 and 3:
table 2: retention rate (%). of the products obtained in examples 1 to 6 and comparative example 1 after standing at ordinary temperature for 3 months
Table 3: the products obtained in examples 1 to 7 and comparative example 1 were left at high temperature for 72h retention (%)
As can be seen from tables 2 and 3, the plant essential oil microcapsule of the present invention has good retention of essential oil with retention rate of more than 99% when placed at room temperature for three months. Standing at high temperature for 72h, wherein the retention rate is more than 85% at 100 ℃; at 130 ℃, the retention rate reaches more than 80 percent; at 160 ℃, the retention rate reaches over 75 percent; in contrast, comparative example 1, which was only subjected to one-time embedding, showed a low retention. Therefore, the secondary embedding of the invention can reduce the volatilization of the essential oil and improve the stability of the essential oil, and particularly has good stability under the condition of high temperature. Therefore, the plant essential oil microcapsule is used for the regenerated cellulose fiber to obtain the long-lasting fragrant regenerated cellulose fiber, and the fragrant regenerated cellulose fiber is woven into the fabric, so that the fabric is used for home textiles, has the effects of soothing the nerves and helping sleep, and still has faint scent after being washed for hundreds of times.
According to the invention, the plant essential oil microcapsules are added into the cellulose spinning solution for spinning to obtain the aromatic regenerated cellulose fibers, and the aromatic regenerated cellulose fibers are taken as raw materials for spinning to form the fabric, so that the fabric not only has the advantages of comfort and skin friendliness of the regenerated cellulose fiber fabric, but also maintains the fragrance of the plant essential oil, and has the effects of soothing the nerves and protecting health. The plant essential oil microcapsule of the invention firstly utilizes the special cavity of the cyclodextrin to wrap the plant essential oil to form the microcapsule on the molecular level, and then wraps the chitosan/sodium alginate biological capsule on the outer side of the cyclodextrin to form the double-layer plant essential oil microcapsule, thereby improving the slow release property and the stability of the microcapsule, and the aromatic regenerated cellulose fiber of the invention has long service life. Therefore, the invention effectively overcomes some practical problems in the prior art, thereby having high utilization value and use significance.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (13)
1. The preparation method of the aromatic regenerated cellulose fiber is characterized by at least comprising the following steps:
preparing plant essential oil microcapsules;
adding the plant essential oil microcapsule, chitosan and a viscose crosslinking agent into a cellulose fiber spinning solution according to a certain proportion, and uniformly stirring to obtain a mixed solution;
spinning the mixed solution to obtain aromatic regenerated cellulose fibers;
the plant essential oil microcapsule is 8-20 parts by mass, the chitosan is 5-10 parts by mass, the viscose crosslinking agent is 2-10 parts by mass, the cellulose fiber spinning solution is 1000 parts by mass, and the content of alpha fibers in the cellulose fiber spinning solution is 8-15 wt%.
2. The method for preparing aromatic regenerated cellulose fiber according to claim 1, characterized in that the preparation of plant essential oil microcapsule comprises the following steps:
preparing a core material solution by using plant essential oil;
preparing a wall material solution by using cyclodextrin;
adding the core material solution into the wall material solution, homogenizing and emulsifying to realize primary embedding of plant essential oil by cyclodextrin;
and carrying out secondary embedding on the plant essential oil by utilizing chitosan/sodium alginate to obtain the double-layer microcapsule.
3. The method of preparing aromatic regenerated cellulose fiber according to claim 2, wherein the step of preparing a core material solution comprises: uniformly mixing plant essential oil and absolute ethyl alcohol according to the mass ratio of 1 (2-5), adding lecithin into the solution, and heating to completely dissolve the lecithin, wherein the mass ratio of the plant essential oil to the lecithin is (1-5) to 2.
4. The method for preparing aromatic regenerated cellulose fiber according to claim 2, characterized in that the step of preparing the wall material solution comprises: adding 60-80 parts by mass of cyclodextrin, 10-25 parts by mass of sodium starch octenyl succinate and 5-12 parts by mass of emulsified modified starch into water, stirring for 1 hour at 50-70 ℃, adding 5-10 parts by mass of emulsifier, mixing and stirring for 20min, wherein the mass ratio of the total mass of the cyclodextrin, the sodium starch octenyl succinate and the emulsified modified starch to the mass of the water is 1:
(4～10)。
5. the method for preparing aromatic regenerated cellulose fiber according to claim 2, characterized in that the cyclodextrin primary entrapment of plant essential oil comprises: adding the core material solution into the wall material solution, and stirring for 20-60 min at 40-60 ℃; and (3) homogenizing and emulsifying the mixed solution of the core material solution and the wall material solution by using a homogenizer to obtain a stable emulsifying system, and drying the stable emulsifying system to obtain the single-layer microcapsule.
6. The method for preparing aromatic regenerated cellulose fiber according to claim 5, characterized in that the homogenizing emulsification comprises a first homogenizing and a second homogenizing, wherein the first homogenizing is performed at 5000-20000 rpm for 5-20 min under 100-500 bar pressure; and the secondary homogenization is to add liquid paraffin into the emulsion obtained by the primary homogenization, and homogenize for 5-20 min again, wherein the addition amount of the liquid paraffin is 0.5-2% of the total mass of the emulsion.
7. The method for preparing aromatic regenerated cellulose fibers according to claim 2, characterized in that the secondary embedding comprises: adding the single-layer microcapsule obtained by primary embedding into a sodium alginate solution, and uniformly stirring at 50-60 ℃ to obtain a mixed solution; adding chitosan and calcium chloride into the mixed solution, stirring uniformly, and carrying out ultrasonic treatment for 5 min; filtering and drying to obtain the double-layer microcapsule.
8. The method for preparing aromatic regenerated cellulose fiber according to claim 7, characterized in that the sodium alginate solution comprises 3-8 wt% of sodium alginate, 2-4 wt% of polyethylene glycol and 1 wt% of dibutyl tin dilaurate; the concentration of the chitosan in the mixed system is 2-3 wt%, and the concentration of the calcium chloride in the mixed system is 0.5-2 wt%.
9. The preparation method of the aromatic regenerated cellulose fibers according to claim 1, characterized in that the viscose cross-linking agent is prepared by diluting the cellulose fiber spinning solution to 5-6 wt% of methyl cellulose, adding 0.1-0.2 wt% of polyacrylamide and 0.1-0.2 wt% of hydrogen peroxide, mixing and stirring uniformly.
10. The method for preparing aromatic regenerated cellulose fibers according to claim 1, characterized in that the cellulose fiber spinning solution is prepared from pulp with a polymerization degree of 500 to 800.
11. The aromatic regenerated cellulose fiber prepared by the preparation method of any one of claims 1 to 10, which is characterized by comprising the following raw material components in parts by weight:
wherein the cellulose content in the cellulose fiber spinning solution is 8-15 wt%.
12. The aromatic regenerated cellulose fiber according to claim 11, wherein the plant essential oil microcapsule comprises a core material, a first wall material and a second wall material, the first wall material is coated on the outer side of the core material, the second wall material is coated on the outer side of the first wall material, the core material is plant essential oil, the first wall material is cyclodextrin, and the second wall material is chitosan/sodium alginate.
13. A fragrant fabric produced by weaving the fragrant regenerated cellulose fiber according to claim 11 or 12.
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| CN116043564A (en) * | 2022-09-16 | 2023-05-02 | 冠和卫生用品有限公司 | Aromatic non-woven fabric based on phase-change microcapsules and preparation method thereof |
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