CN112323160A - LYOCELL fiber containing plant active ingredients and preparation method thereof - Google Patents
LYOCELL fiber containing plant active ingredients and preparation method thereof Download PDFInfo
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- CN112323160A CN112323160A CN202011234929.2A CN202011234929A CN112323160A CN 112323160 A CN112323160 A CN 112323160A CN 202011234929 A CN202011234929 A CN 202011234929A CN 112323160 A CN112323160 A CN 112323160A
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- 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
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- 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
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Abstract
The invention discloses a LYOCELL fiber containing plant active ingredients and a preparation method thereof, relating to the technical field of fibers, and the key points of the technical scheme are as follows: a method for preparing LYOCELL fiber containing plant active ingredients comprises the following steps: s1, preparing an active agent containing plant active ingredients; s2, preparing a cellulose dissolving solution; s3, mixing; and S4, spinning. The preparation method of the invention endows the LYOCELL fiber with multiple functions and durable performance by a wrapping and grafting dual method. In addition, the LYOCELL fiber containing plant active ingredients prepared by the preparation method has the advantages of multiple functions, high tensile strength and durability.
Description
Technical Field
The invention relates to the field of fiber, in particular to LYOCELL fiber containing plant active ingredients and a preparation method thereof.
Background
The LYOCELL fiber is prepared by dissolving wood (mainly eucalyptus) pulp in organic solvent N-methylmorpholine-N-oxide, and spinning by dry-jet wet method; and the generated cellulose fiber has the advantages of high dry strength and wet strength, good washing stability, excellent hygroscopicity, soft hand feeling and the like. Therefore, LYOCELL fiber is popular among consumers and widely used in various fields due to its advantages of wide raw material source, simple spinning process, recyclable solvent, excellent performance of the obtained fiber, etc. The plant active ingredients refer to substances which form the plant body, besides essential substances such as moisture, saccharides, proteins, fats and the like, the plant active ingredients also comprise secondary metabolites (such as terpenes, flavones, alkaloids, steroids, lignin, minerals and the like), and the substances have physiological promotion effects on human beings and various organisms.
In the prior art, reference is made to patent document with an authorization publication number of CN103966685B, which discloses a skin-soothing plant fiber fabric, which is prepared from the following raw materials in parts by weight: 100-120 parts of 1-ethyl-3-methylimidazole acetate, 4-5 parts of nano chitin, 1-2 parts of jojoba oil, 8-10 parts of water, 7-10 parts of plastic starch, 2-4 parts of polycaprolactone, 1-2 parts of white oil, 1-2 parts of vitamin E, 3-4 parts of lavender, 4-6 parts of rosemary, 10-14 parts of silk fiber, 54-58 parts of ramie fiber, 25-27 parts of banana fiber and 0.4-0.8 part of spinning auxiliary agent; the ramie fiber raw material is used in the fabric, so that the fabric has the performances of bacteriostasis, ventilation, coolness, corrosion prevention, mildew prevention and sweat absorption, and the glossiness and softness of the fiber are increased by matching the banana fiber and the silk fiber; vitamin E, lavender and rosemary are added, so that the skin can be relieved, the grease secretion can be balanced, and the acne and inflammation can be resisted; said invented spinning adjuvant can make spinning melt obtain good spinnability, and can make fibre have no broken filament, and can be uniformly dyed, and its colour and lustre are good and hand feeling is soft.
However, the functional components in the fabric, such as banana fiber, silk fiber, vitamin E, lavender, rosemary, and the like, are added to the ramie fibers by physical mixing, so that the bonding force between the functional components and the ramie fibers is weak, and the functional components are easily separated from the ramie fibers when the fabric is subjected to mechanical friction, repeated washing or high temperature and acid-base environments for a long time, so that the functionality of the manufactured plant fiber fabric is reduced, and the service cycle of the plant fiber fabric is further shortened.
Disclosure of Invention
In view of the deficiencies of the prior art, a first object of the present invention is to provide a method for preparing LYOCELL fibers containing plant active ingredients, which provides the LYOCELL fibers with versatility and durability through a dual process of wrapping and grafting.
It is a second object of the present invention to provide LYOCELL fibers containing plant active ingredients that have the advantages of versatility, high tensile strength, and durability.
In order to achieve the first object, the invention provides the following technical scheme: a method for preparing LYOCELL fiber containing plant active ingredients comprises the following steps:
s1, preparing an active agent containing plant active ingredients;
s2, preparing a cellulose dissolving solution:
s21, weighing: weighing a certain amount of cellulose pulp;
s22, enzyme activation: adding complex enzyme into the cellulose pulp weighed in the step S21 for enzyme activation to obtain a cellulose activator;
s23, drying: inactivating enzyme, filtering and drying the cellulose activator obtained in the step S22 to obtain a dried cellulose;
s24, dissolving cellulose: mixing the dried fiber obtained in the step S23, 50 wt% of N-methylmorpholine-N-oxide solution and an antioxidant according to a mass ratio of 10-15: 100:1, mixing, heating, decompressing and dehydrating to prepare a cellulose dissolving solution;
s3, mixing: adding the active agent prepared in the preparation S1 into the cellulose dissolving solution prepared in the preparation S2, and adding K2S2O8And aziridine crosslinking agent, dispersing by ultrasonic at 55-60 deg.C, and reacting at 55 deg.C for 5-6h to obtain spinning solution containing plant active components;
s4, spinning: spinning the spinning solution obtained in the step S3 to obtain LYOCELL fiber containing plant active ingredients.
By adopting the technical scheme, active groups contained in substances such as terpenes, phenols and the like in the active agent prepared by extracting the plant active ingredients have strong reactivity and K is higher than K2S2O8And aziridine crosslinking agent, so that the functional group can be grafted and copolymerized with hydroxyl in cellulose molecules, thereby endowing the cellulose molecules with diversified functionality. In addition, the method of chemical grafting can improve the binding firmness of the plant active substance and the cellulose molecules, and reduce the separation of the active substance and the cellulose molecules, thereby ensuring that the functionality of the LYOCELL fiber is more durable; the graft copolymerization is continuously carried out between the cellulose molecules after the graft copolymerization, thereby forming an intricate cross-linked network structure, improving the performance of the LYOCELL fiber in all aspects, improving the mechanical property of the LYOCELL fiber, and further prolonging the service life of the LYOCELL fiber.
Furthermore, the preparation method of the LYOCELL fiber containing the plant active ingredients is characterized in that the dosage form of the active agent is one of nano sustained-release capsules, nano sustained-release microspheres and nano sustained-release liposomes.
By adopting the technical scheme, the organic solvent N-methylmorpholine-N-oxide used in the preparation process of the LYOCELL fiber has oxidability, and can easily oxidize the plant active ingredients to denature and inactivate the plant active ingredients. Therefore, in order to protect the activity of the plant active ingredients, the plant active ingredients are coated to prepare a slow-release capsule, and then the slow-release capsule is combined with cellulose molecules in the spinning solution through a graft copolymerization process, so that the plant active capsules are firmly combined on the cellulose molecules, and the plant active ingredients are favorably and firmly attached to the cellulose molecules. Therefore, by using the method of wrapping and graft copolymerization on the plant active ingredients, the plant active ingredients are effectively protected, the binding firmness of the active substances and cellulose molecules is improved, the separation of the active substances and the cellulose molecules is reduced, the functionality of the LYOCELL fiber is more durable, and the service cycle of the LYOCELL fiber is further prolonged.
Further, the active agent, the cellulose dissolving solution, and K in the step S32S2O8And the aziridine crosslinking agent in a weight ratio of 2-3:100: 1: 1.
by adopting the technical scheme, the addition amount of the active agent is small, so that the functionality is not obvious, but the addition amount of the active agent is large, so that the roughness of the surface of the LYOCELL fiber is increased; thus, the active agent, the cellulose dissolving solution and K are mixed2S2O8And the mass ratio of the aziridine crosslinking agent to the aziridine crosslinking agent is controlled to be 2-3:100: 1:1, the LYOCELL fiber can be endowed with excellent functionality and maintain the original silky smooth performance of the LYOCELL fiber.
Further, the active agent in the step S1 is prepared from the following raw materials in parts by weight: 3-5 parts of plant active ingredients, 12-16 parts of chitosan, 403-5 parts of castor oil polyoxyethylene ether EL, and 0.8-1.2 parts of 1 wt% sodium tripolyphosphate solution.
By adopting the technical scheme, the amino group with positive charge on the chitosan molecule and the phosphate radical with negative charge on the sodium tripolyphosphate can be mutually crosslinked under the action of the aziridine crosslinking agent sodium tripolyphosphate through electrostatic interaction to obtain the blank nano slow-release microcapsules, and the blank nano slow-release microcapsules and the plant active ingredients are subjected to ion gelation, so that the plant active ingredients are coated to prepare the nano slow-release capsules.
Further, the active agent is in the form of a nano sustained-release capsule, and the preparation process of the nano sustained-release capsule comprises the following steps:
step 1, weighing: 3-5 parts of plant active ingredients, 12-16 parts of chitosan, 403-5 parts of castor oil polyoxyethylene ether EL and 0.8-1.2 parts of 1 wt% sodium tripolyphosphate solution are respectively weighed according to parts by weight;
step 2, preparing a blank nano sustained-release capsule:
step 21, dissolving chitosan in 1 wt% of glacial acetic acid to prepare 0.5 wt% of chitosan solution, uniformly stirring at the temperature of 55-60 ℃, and then adjusting the pH value to 5 to obtain solution A;
step 22, adding castor oil polyoxyethylene ether EL40 into the solution A in the step 21, uniformly stirring at the temperature of 55-60 ℃, and then cooling to room temperature to obtain a solution B;
step 3, preparing a solution containing plant active ingredients: dissolving plant active ingredients in absolute ethyl alcohol, and uniformly stirring at room temperature to prepare a 5 wt% plant active ingredient solution;
step 4, adding the 5 wt% of plant active ingredient solution prepared in the step 3 into the solution B in the step 22, and uniformly stirring at room temperature to obtain a solution C;
step 5, dropwise adding 1 wt% sodium tripolyphosphate solution into the solution C at the speed of 0.02mL/s, and stirring at the stirring speed of 500r/min for 60-80min at room temperature to form a nanocapsule dispersion liquid;
and 6, centrifuging the nano-capsule dispersion liquid obtained in the step 5 at 10000rpm for 20-30min, and then taking supernatant liquid to obtain the active agent through ultrasonic dispersion.
By adopting the technical scheme, the blank nano microcapsule is formed by crosslinking through the electrostatic action of anions carried by cationic sodium pre-tripolyphosphate carried by the amino group of chitosan; then mixing the blank nano microcapsule with a solution containing plant active ingredients to ensure that the blank nano slow-release microcapsule and the plant active ingredients are subjected to ion gelation, thereby coating the plant active ingredients to prepare a nano capsule slow-release dispersion liquid; then large particle substances which affect the smoothness of LYOCELL fibers can be removed by centrifugation; the nano-level nano sustained-release capsule has obvious agglomeration phenomenon, so the nano-level nano sustained-release capsule needs to be fully dispersed after ultrasonic dispersion, thereby improving the uniformity after being added into cellulose.
Further, the ultrasonic dispersion power in the step 6 is 300w, and the ultrasonic dispersion time is 10-12 min.
By adopting the technical scheme, the nano sustained-release capsule preparation is easy to crack due to overhigh ultrasonic dispersion power and overhigh temperature of a solution system caused by overlong ultrasonic dispersion time, so that the coating rate of the nano sustained-release capsule is reduced; therefore, through low-power and long-time ultrasonic dispersion, the high coating rate of the nano sustained-release capsules can be ensured, and the uniform dispersion of the nano sustained-release capsules is facilitated.
Further, the ultrasonic dispersion power in the step S3 is 400w and the ultrasonic dispersion time is 15-20 min.
By adopting the technical scheme, the conditions that the viscosity of the cellulose dissolving solution is high and the nano sustained-release capsule is easy to break under the condition of high ultrasonic dispersion power are considered; therefore, the ultrasonic dispersion power is 400w, the ultrasonic dispersion is 15-20min, the high coating rate of the nano sustained-release capsule and the dispersion uniformity in the cellulose dissolving solution can be effectively ensured, and the suitable conditions of the graft polymerization between the nano sustained-release capsule and cellulose molecules are also ensured.
Further, the following processing is added after the step 6: step 7, adding 40 wt% of sodium hydroxide solution and chloroacetic acid into the active agent, wherein the weight ratio of the nano sustained-release capsule, the 40 wt% of sodium hydroxide solution and the chloroacetic acid is 20: 100:1, reacting for 60-80min at 0-5 ℃ to prepare the carboxymethyl activating agent.
By adopting the technical scheme, the chitosan is highly insoluble due to the strong hydrogen bond effect in the chitosan molecules in the capsule wall components of the nano sustained-release capsule, so that the prepared nano sustained-release capsule is also highly insoluble, the combination of the nano sustained-release capsule and cellulose molecules is insufficient, and the effect of graft polymerization is influenced; therefore, hydroxyl on chitosan molecules reacts with chloroacetic acid in an alkaline environment, and a carboxymethyl is introduced to form a carboxylate structure with strong polarity which can be directly dissolved in water, so that the solubility of the chitosan is improved, and the introduced carboxylate structure can be combined with the hydroxyl on cellulose molecules, thereby being beneficial to enhancing the combination of the nano sustained-release capsule and the cellulose.
In order to achieve the second object, the invention provides the following technical scheme: a LYOCELL fiber containing plant active ingredients is prepared by the above method.
By adopting the technical scheme, the LYOCELL fiber prepared by the preparation method has the advantages of multiple functions, high tensile strength and durability.
In conclusion, the invention has the following beneficial effects:
firstly, the method of the invention not only can endow the LYOCELL fiber with multiple functions by a chemical grafting method; but also can improve the combination firmness of the plant active substance and the cellulose molecules and reduce the separation of the active substance and the cellulose molecules, thereby ensuring that the LYOCELL fiber has more durable functionality; the graft copolymerization is continuously carried out between the cellulose molecules after the graft copolymerization, thereby forming an intricate cross-linked network structure, being beneficial to improving various performances of the LYOCELL fiber, and further prolonging the service time of the LYOCELL fiber.
Secondly, the invention preferably adopts a method of wrapping and graft copolymerization on the plant active ingredients, which not only effectively protects the plant active ingredients, but also improves the bonding firmness of the active substances and the cellulose molecules, reduces the separation of the active substances and the cellulose molecules, thereby ensuring the functions of the LYOCELL fiber to be more durable and further prolonging the service cycle of the LYOCELL fiber.
Thirdly, the LYOCELL fiber prepared by the invention has the advantages of multifunction, high tensile strength and durability.
Detailed Description
The present invention will be described in further detail with reference to examples.
Preparation of active agent
The plant active component in the preparation example of the active agent can be one or more of mint extract, sarcandra glabra extract, apocynum venetum extract, wormwood extract, isatis root extract, motherwort extract, lavender extract and tea extract; in each preparation example of the active agent, the plant active ingredients are prepared by mixing commercially available mint extract, sarcandra glabra extract and lavender extract, and the mass ratio of the mint extract to the sarcandra glabra extract to the lavender extract is 1: 1; the chitosan is commercially available chitosan, the content of the chitosan is more than or equal to 99 percent, and the chitosan is white crystalline powder; the castor oil polyoxyethylene ether EL40 is commercially available castor oil polyoxyethylene ether EL40, the content of which is more than or equal to 99 percent, and the castor oil polyoxyethylene ether EL40 is light yellow oily paste.
Preparation of active agent example 1
Step 1, weighing: weighing 3 parts of plant active ingredients by weight;
step 2, dissolving: dissolving the plant active ingredients weighed in the step 1 in absolute ethyl alcohol, wherein the volume ratio of the plant active ingredients to the absolute ethyl alcohol is 1:5, and stirring at the stirring speed of 200r/min for 10min at room temperature to obtain the active agent.
Preparation example 2 of active agent
Step 1, weighing: 3 parts of plant active ingredients, 12 parts of chitosan, 403 parts of castor oil polyoxyethylene ether EL and 0.8 part of 1 wt% sodium tripolyphosphate solution are respectively weighed according to parts by weight;
step 2, preparing a blank nano sustained-release capsule:
step 21, dissolving chitosan in 1 wt% of glacial acetic acid to prepare 0.5 wt% of chitosan solution, stirring for 20min at a stirring speed of 200r/min at the temperature of 55 ℃, uniformly stirring, and then adjusting the pH value to 5 to obtain solution A;
step 22, adding castor oil polyoxyethylene ether EL40 into the solution A in the step 21, stirring for 30min at the stirring speed of 200r/min at the temperature of 55 ℃, uniformly stirring, and then cooling to room temperature to obtain a solution B;
step 3, preparing a solution containing plant active ingredients: dissolving plant active ingredients in anhydrous ethanol, stirring at room temperature at a stirring rate of 200r/min for 20min, and stirring to obtain 5 wt% plant active ingredient solution;
step 4, adding the 5 wt% of plant active ingredient solution prepared in the step 3 into the solution B in the step 22, stirring for 40min at the stirring speed of 200r/min at room temperature, and uniformly stirring to obtain a solution C;
step 5, dropwise adding a 1 wt% sodium tripolyphosphate solution into the solution C at a speed of 0.02mL/s, and stirring at a stirring speed of 500r/min for 60min at room temperature to form a nanocapsule dispersion liquid;
and 6, centrifuging the nano-capsule dispersion liquid obtained in the step 5 at 10000rpm for 20min, and then taking the supernatant to perform ultrasonic dispersion, wherein the ultrasonic power is controlled to be 300w and the ultrasonic dispersion time is controlled to be 10min in the ultrasonic dispersion process to obtain the active agent.
Preparation of active agent example 3
Step 1, weighing: respectively weighing 4 parts of plant active ingredients, 14 parts of chitosan, 404 parts of castor oil polyoxyethylene ether EL and 1 part of 1 wt% sodium tripolyphosphate solution according to parts by weight;
step 2, preparing a blank nano sustained-release capsule:
step 21, dissolving chitosan in 1 wt% of glacial acetic acid to prepare 0.5 wt% of chitosan solution, stirring for 20min at a stirring speed of 200r/min at the temperature of 55 ℃, uniformly stirring, and then adjusting the pH value to 5 to obtain solution A;
step 22, adding castor oil polyoxyethylene ether EL40 into the solution A in the step 21, stirring for 30min at the stirring speed of 200r/min at the temperature of 55 ℃, uniformly stirring, and then cooling to room temperature to obtain a solution B;
step 3, preparing a solution containing plant active ingredients: dissolving plant active ingredients in anhydrous ethanol, stirring at room temperature at a stirring rate of 200r/min for 20min, and stirring to obtain 5 wt% plant active ingredient solution;
step 4, adding the 5 wt% of plant active ingredient solution prepared in the step 3 into the solution B in the step 22, stirring for 40min at the stirring speed of 200r/min at room temperature, and uniformly stirring to obtain a solution C;
step 5, dropwise adding a 1 wt% sodium tripolyphosphate solution into the solution C at a speed of 0.02mL/s, and stirring at a stirring speed of 500r/min for 70min at room temperature to form a nanocapsule dispersion liquid;
and 6, centrifuging the nano-capsule dispersion liquid obtained in the step 5 at 10000rpm for 25min, and then taking the supernatant to perform ultrasonic dispersion, wherein the ultrasonic power is controlled to be 300w and the ultrasonic dispersion time is controlled to be 10min in the ultrasonic dispersion process to obtain the active agent.
Preparation of active agent example 4
Step 1, weighing: respectively weighing 5 parts of plant active ingredients, 16 parts of chitosan, 405 parts of castor oil polyoxyethylene ether EL and 1.2 parts of 1 wt% sodium tripolyphosphate solution according to parts by weight;
step 2, preparing a blank nano sustained-release capsule:
step 21, dissolving chitosan in 1 wt% of glacial acetic acid to prepare 0.5 wt% of chitosan solution, stirring for 20min at a stirring speed of 200r/min at the temperature of 55 ℃, uniformly stirring, and then adjusting the pH value to 5 to obtain solution A;
step 22, adding castor oil polyoxyethylene ether EL40 into the solution A in the step 21, stirring for 30min at the stirring speed of 200r/min at the temperature of 55 ℃, uniformly stirring, and then cooling to room temperature to obtain a solution B;
step 3, preparing a solution containing plant active ingredients: dissolving plant active ingredients in anhydrous ethanol, stirring at room temperature at a stirring rate of 200r/min for 20min, and stirring to obtain 5 wt% plant active ingredient solution;
step 4, adding the 5 wt% of plant active ingredient solution prepared in the step 3 into the solution B in the step 22, stirring for 40min at the stirring speed of 200r/min at room temperature, and uniformly stirring to obtain a solution C;
step 5, dropwise adding a 1 wt% sodium tripolyphosphate solution into the solution C at a speed of 0.02mL/s, and stirring at a stirring speed of 500r/min for 80min at room temperature to form a nanocapsule dispersion liquid;
and 6, centrifuging the nano-capsule dispersion liquid obtained in the step 5 at 10000rpm for 30min, and then taking the supernatant to perform ultrasonic dispersion, wherein the ultrasonic power is controlled to be 300w and the ultrasonic dispersion time is 12min in the ultrasonic dispersion process to obtain the active agent.
Preparation of active agent example 5
The difference between the preparation example and the preparation example 2 of the active agent is that the preparation example is provided with a step 7, 40 wt% of sodium hydroxide solution and chloroacetic acid are added into the active agent, and the weight ratio of the nano sustained-release capsule, the 40 wt% of sodium hydroxide solution and the chloroacetic acid is 20: 100:1, reacting for 60min at 5 ℃ to prepare the carboxymethyl activating agent.
Comparative examples of active Agents
This comparative example differs from preparation example 2 of an active agent in that step 6 is not provided in this preparation example.
The cellulose pulp in the examples includes, but is not limited to, wood pulp, having a degree of polymerization of about 547, and an alpha-cellulose mass fraction of 88%; the content of N-methylmorpholine-N-oxide is 50 percent; the compound enzyme comprises cellulase and pectinase in a mass ratio of 2:1, wherein the cellulase is commercially available cellulase with the content of 99 percent and the enzyme activity of 2 ten thousand U/g, and the pectinase is commercially available pectinase with the content of 99 percent and the enzyme activity of 5 ten thousand U/g; the antioxidant is propyl gallate with a content of 99%.
Example 1
S1, preparing an active agent containing plant active ingredients;
s2, preparing a cellulose dissolving solution:
s21, weighing: weighing 1000 parts of cellulose pulp;
s22, enzyme activation: adding complex enzyme with the mass being 1% of the mass of the cellulose pulp into the cellulose pulp weighed in the step S21 to carry out enzyme activation for 80min to obtain a cellulose activator;
s23, drying: inactivating enzyme of the cellulose activator obtained in the step S22 at 100 ℃ for 40min, filtering, taking supernatant, and drying the supernatant at 60 ℃ for 60min to obtain a dried cellulose;
s24, dissolving cellulose: mixing the dried fiber obtained in the step S23, 50 wt% of N-methylmorpholine-N-oxide solution and an antioxidant according to a mass ratio of 10: 100:1, mixing; then stirring for 15min at the stirring speed of 50r/min at room temperature and normal pressure; then heating to 90 ℃, decompressing to 0.2MPa, stirring at the stirring speed of 200r/min for 60min, dehydrating and dissolving to prepare cellulose dissolving solution;
s3, mixing: adding the active agent prepared in the step S1 to the cellulose dissolving solution prepared in the step S2, and adding K2S2O8And aziridine crosslinking agent, and active agent, cellulose solution, K2S2O8And aziridine crosslinking agent in a weight ratio of 2:100: 1:1, then dispersing the mixture by ultrasonic waves at the temperature of 55 ℃, controlling the ultrasonic dispersion power to be 400w in the ultrasonic dispersion process and carrying out ultrasonic dispersionThe time is 15min, and then the reaction is carried out for 5h under the condition of keeping the temperature at 55 ℃ to prepare spinning solution containing plant active ingredients;
s4, spinning: and (4) spinning the spinning solution obtained in the step (S3), wherein the spinning speed is controlled to be 60m/min, the spinning air gap is 30mm, the spinning blowing temperature is 20 ℃, the spinning blowing flow is 400L/H, the blowing relative humidity is 60%, the coagulation bath mass concentration is 20%, and the coagulation bath temperature is 25 ℃ in the spinning process, so that the LYOCELL fiber containing the plant active ingredients is obtained.
The active agent used in this example was prepared in preparation example 1 of the active agent.
Example 2
S1, preparing an active agent containing plant active ingredients;
s2, preparing a cellulose dissolving solution:
s21, weighing: weighing 1000 parts of cellulose pulp;
s22, enzyme activation: adding complex enzyme with the mass being 1% of the mass of the cellulose pulp into the cellulose pulp weighed in the step S21 to carry out enzyme activation for 80min to obtain a cellulose activator;
s23, drying: inactivating enzyme of the cellulose activator obtained in the step S22 at 100 ℃ for 40min, filtering, taking supernatant, and drying the supernatant at 60 ℃ for 60min to obtain a dried cellulose;
s24, dissolving cellulose: mixing the dried fiber obtained in the step S23, 50 wt% of N-methylmorpholine-N-oxide solution and an antioxidant according to a mass ratio of 10: 100:1, mixing; then stirring for 15min at the stirring speed of 50r/min at room temperature and normal pressure; then heating to 90 ℃, decompressing to 0.2MPa, stirring at the stirring speed of 200r/min for 60min, dehydrating and dissolving to prepare cellulose dissolving solution;
s3, mixing: adding the active agent prepared in the step S1 to the cellulose dissolving solution prepared in the step S2, and adding K2S2O8And aziridine crosslinking agent, and active agent, cellulose solution, K2S2O8And aziridine crosslinking agent in a weight ratio of 2.5:100:1:1, ultrasonic dispersing at 55 deg.C, and ultrasonic dispersingControlling the ultrasonic dispersion power to be 400w and the ultrasonic dispersion time to be 18min in the acoustic dispersion process, and then reacting for 5h under the condition of keeping the temperature to be 55 ℃ to prepare spinning solution containing plant active ingredients;
s4, spinning: and (4) spinning the spinning solution obtained in the step (S3), wherein the spinning speed is controlled to be 60m/min, the spinning air gap is 30mm, the spinning blowing temperature is 20 ℃, the spinning blowing flow is 400L/H, the blowing relative humidity is 60%, the coagulation bath mass concentration is 20%, and the coagulation bath temperature is 25 ℃ in the spinning process, so that the LYOCELL fiber containing the plant active ingredients is obtained.
The active agent used in this example was prepared in preparation example 1 of the active agent.
Example 3
S1, preparing an active agent containing plant active ingredients;
s2, preparing a cellulose dissolving solution:
s21, weighing: weighing 1000 parts of cellulose pulp;
s22, enzyme activation: adding complex enzyme with the mass being 1% of the mass of the cellulose pulp into the cellulose pulp weighed in the step S21 to carry out enzyme activation for 80min to obtain a cellulose activator;
s23, drying: inactivating enzyme of the cellulose activator obtained in the step S22 at 100 ℃ for 40min, filtering, taking supernatant, and drying the supernatant at 60 ℃ for 60min to obtain a dried cellulose;
s24, dissolving cellulose: mixing the dried fiber obtained in the step S23, 50 wt% of N-methylmorpholine-N-oxide solution and an antioxidant according to a mass ratio of 10: 100:1, mixing; then stirring for 15min at the stirring speed of 50r/min at room temperature and normal pressure; then heating to 90 ℃, decompressing to 0.2MPa, stirring at the stirring speed of 200r/min for 60min, dehydrating and dissolving to prepare cellulose dissolving solution;
s3, mixing: adding the active agent prepared in the step S1 to the cellulose dissolving solution prepared in the step S2, and adding K2S2O8And aziridine crosslinking agent, and active agent, cellulose solution, K2S2O8And aziridine crosslinking agent in a weight ratio of 3:100:1:1, then dispersing by ultrasonic waves at the temperature of 55 ℃, controlling the ultrasonic dispersion power to be 400w and the ultrasonic dispersion time to be 20min in the ultrasonic dispersion process, and then reacting for 6h under the condition of keeping the temperature of 55 ℃ to prepare spinning solution containing plant active ingredients;
s4, spinning: and (4) spinning the spinning solution obtained in the step (S3), wherein the spinning speed is controlled to be 60m/min, the spinning air gap is 30mm, the spinning blowing temperature is 20 ℃, the spinning blowing flow is 400L/H, the blowing relative humidity is 60%, the coagulation bath mass concentration is 20%, and the coagulation bath temperature is 25 ℃ in the spinning process, so that the LYOCELL fiber containing the plant active ingredients is obtained.
The active agent used in this example was prepared in preparation example 1 of the active agent.
Example 4
This example is different from example 1 in that the active agent used in this example was prepared in preparation example 2 of the active agent.
Example 5
This example is different from example 1 in that the active agent used in this example was prepared in preparation example 3 of an active agent.
Example 6
This example is different from example 1 in that the active agent used in this example was prepared in preparation example 4 of an active agent.
Example 7
This example is different from example 1 in that the active agent used in this example was prepared in preparation example 5 of an active agent.
Comparative example
Comparative example 1
This comparative example differs from example 4 in that the active agent used in this comparative example is a comparative example of an active agent.
Comparative example 2
This comparative example differs from example 4 in that step S3, mixing: adding the active agent prepared in the step S1 into the cellulose dissolving solution prepared in the step S2, wherein the weight ratio of the active agent to the cellulose dissolving solution is 2:100, then carrying out ultrasonic dispersion at the temperature of 80 ℃, and controlling the ultrasonic dispersion power to be 400w and the ultrasonic dispersion time to be 15min in the ultrasonic dispersion process to prepare the spinning solution containing the plant active ingredients.
Comparative example 3
This comparative example differs from example 4 in that it was selected from a commercially available LYOCELL fiber; the LYOCELL fiber is LYOCELL bamboo knitted fabric provided by Shanghai Changjie textile Co., Ltd, with the product number CJ-10068.
Detecting items:
(I) detecting the apparent form of the active agent:
1. morphology detection of active agents: the active agents prepared in preparation examples 1 to 5 of the active agent and the active agents prepared in the comparative examples of the active agent were naturally dried at room temperature, and morphological observation was performed by a scanning electron microscope, and the observation results are shown in table 1:
2. detecting the particle size distribution of the active agent: the active agents prepared in preparation examples 1 to 5 of the active agent and the active agent prepared in the comparative example of the active agent were subjected to particle size measurement by a nanometer particle size analyzer (supplied by Chantaylor, model number Winner802), and the measurement results are shown in Table 1:
table 1 apparent morphology assay results for active agents
| Test items | Distribution form of active ingredients | Average particle diameter (nm) of active ingredient |
| Preparation of active agent example 1 | Irregularly shaped particles | Non-uniform in dimension |
| Preparation example 2 of active agent | Full spherical particles with dispersion shape between particles | 173 |
| Preparation of active agent example 3 | Full spherical particles with dispersion shape between particles | 170 |
| Preparation of active agent example 4 | Full spherical particles with dispersion shape between particles | 170 |
| Preparation of active agent example 5 | Full spherical particles with dispersion shape between particles | 175 |
| Comparative examples of active Agents | Spherical particles but with agglomeration between particles | Non-uniform in dimension |
As can be seen from Table 1, the distribution forms of the active ingredients prepared in preparation examples 2-5 of the active agent are all full spherical particles, the particles are dispersed, and the average particle size of the active ingredient is between 170-175nm, which indicates that the active agent prepared by the method has a nano-grade and regular-shaped capsule, and a plurality of capsules are fully dispersed and basically have no agglomeration, thereby being beneficial to the uniform dispersion of the capsules in the system. Compared with the preparation example 2 of the active agent, the active ingredient in the comparative example of the active agent is spherical particles, but the particles are agglomerated, so that the shape and the size are irregular, and the ultrasonic dispersion is favorable for eliminating the agglomeration phenomenon in nano-sized capsules and fully dispersing the capsules, so that the capsules are favorable for uniformly and fully combining the capsules and cellulose, and the functionality and the durability of the prepared LYOCELL fiber are improved.
And (II) detecting the performance of LYOCELL fiber:
1. and (3) stretching detection: after LYOCELL fibers prepared in examples 1-7 and LYOCELL fibers prepared in comparative examples 1-3 were prepared into LYOCELL fabrics by a LYOCELL fiber production line, the fabrics were prepared according to GB/T3923.1-2013 part 1 of tensile Properties of textile fabrics: measurement of breaking strength and elongation at break (bar method) the measurement results of LYOCELL fabric are shown in Table 2:
2. and (3) detecting the tearing performance: after the LYOCELL fibers prepared in examples 1-7 and the LYOCELL fibers prepared in comparative examples 1-3 were prepared into LYOCELL fabric by a LYOCELL fiber production line, the fabric was torn according to GB/T3917.1-2009 part 1 of textile fabric tear Performance: measurement of tear Strength by impact pendulum method LYOCELL fabric was measured, and the results are shown in Table 2:
TABLE 2LYOCELL fiber Performance test results
As can be seen from Table 2, the LYOCELL fibers prepared in examples 1-7 are superior to the LYOCELL fibers prepared in comparative example 3 in properties of breaking strength, elongation at break and tearing strength, compared with the existing LYOCELL fibers, the LYOCELL fibers prepared in examples 1-7 have greatly improved properties of breaking strength, elongation at break and tearing strength, and the active ingredients in the active agent can be graft-copolymerized with cellulose molecules under the action of the initiator, so that the bonding firmness of the plant active substances and the cellulose molecules is improved, the active substances and the cellulose molecules are reduced to be separated, and thus a complex cross-linked network structure is formed, thereby facilitating the improvement of various properties of the LYOCELL fibers and further prolonging the service life of the LYOCELL fibers.
Compared with example 1, the properties of the LYOCELL fiber prepared in example 4 in breaking strength, breaking elongation and tearing strength are superior to those of the LYOCELL fiber prepared in example 1, which shows that the invention not only effectively protects the plant active ingredient, but also improves the binding firmness of the active substance and the cellulose molecules and reduces the separation of the active substance and the cellulose molecules by performing the double actions of wrapping and graft copolymerization on the plant active ingredient, so that the functionality of the LYOCELL fiber is more durable, and the service life of the LYOCELL fiber is further prolonged.
Compared with example 4, the properties of the LYOCELL fiber prepared in example 7 in breaking strength, elongation at break and tearing strength are superior to those of the LYOCELL fiber prepared in example 4, which shows that carboxyl groups on chitosan molecules react with chloroacetic acid in an alkaline environment, and carboxyl methyl groups are introduced to form a carboxylate structure with strong polarity, so that the carboxylate structure can be directly dissolved in water, thus not only improving the solubility of chitosan, but also facilitating the graft polymerization of the nano sustained-release capsules and the hydroxyl groups on cellulose molecules.
Compared with the comparative example 1, the LYOCELL fiber prepared in the example 4 has better properties in breaking strength, breaking elongation and tearing strength than the LYOCELL fiber prepared in the comparative example 1, and the ultrasonic dispersion is favorable for eliminating the agglomeration phenomenon in nano-sized capsules and fully dispersing the capsules, so that the capsules are favorably and uniformly dispersed in a cellulose dissolving solution, and the functionality of the LYOCELL fiber is favorably improved.
Compared with the comparative example 2, the LYOCELL fiber prepared in the example 4 has better properties of breaking strength, breaking elongation and tearing strength than the LYOCELL fiber prepared in the comparative example 2, and compared with the conventional physical dispersion, the active ingredient is in favor of improving the combination firmness of the plant active substance and the cellulose molecules through graft copolymerization between the active ingredient and the cellulose molecules, and reducing the separation of the active substance and the cellulose molecules, thereby forming a complicated cross-linked network structure, being in favor of improving various properties of the LYOCELL fiber, and further prolonging the service time of the LYOCELL fiber.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (8)
1. A method for preparing LYOCELL fiber containing plant active ingredients comprises the following steps:
s1, preparing an active agent containing plant active ingredients;
s2, preparing a cellulose dissolving solution:
s21, weighing: weighing a certain amount of cellulose pulp;
s22, enzyme activation: adding complex enzyme into the cellulose pulp weighed in the step S21 for enzyme activation to obtain a cellulose activator;
s23, drying: inactivating enzyme, filtering and drying the cellulose activator obtained in the step S22 to obtain a dried cellulose;
s24, dissolving cellulose: mixing the dried fiber obtained in the step S23, 50 wt% of N-methylmorpholine-N-oxide solution and an antioxidant according to a mass ratio of 10-15: 100:1, mixing, heating, decompressing and dehydrating to prepare a cellulose dissolving solution;
s3, mixing: adding the active agent prepared in the preparation S1 into the cellulose dissolving solution prepared in the preparation S2, and adding K2S2O8And aziridine crosslinking agent, dispersing by ultrasonic at 55-60 deg.C, and reacting at 55 deg.C for 5-6h to obtain spinning solution containing plant active components;
s4, spinning: spinning the spinning solution obtained in the step S3 to obtain LYOCELL fiber containing plant active ingredients.
2. Root of herbaceous plantThe method of claim 1, wherein the step S3 comprises the steps of applying the active agent, the solution of cellulose, and K2S2O8And aziridine crosslinking agent in a weight ratio of 2-3:100: 1: 1.
3. the method of claim 1 or 2, wherein the active agent is in the form of one of a nano-sustained release capsule, a nano-sustained release microsphere, or a nano-sustained release liposome.
4. The method of claim 3, wherein the active agent is in the form of a nano-sustained release capsule, and wherein the process of preparing the nano-sustained release capsule comprises the steps of:
step 1, weighing: 3-5 parts of plant active ingredients, 12-16 parts of chitosan, 403-5 parts of castor oil polyoxyethylene ether EL and 0.8-1.2 parts of 1 wt% sodium tripolyphosphate solution are respectively weighed according to parts by weight;
step 2, preparing a blank nano sustained-release capsule:
step 21, dissolving chitosan in 1 wt% of glacial acetic acid to prepare 0.5 wt% of chitosan solution, uniformly stirring at the temperature of 55-60 ℃, and then adjusting the pH value to 5 to obtain solution A;
step 22, adding castor oil polyoxyethylene ether EL40 into the solution A in the step 21, uniformly stirring at the temperature of 55-60 ℃, and then cooling to room temperature to obtain a solution B;
step 3, preparing a solution containing plant active ingredients: dissolving plant active ingredients in absolute ethyl alcohol, and uniformly stirring at room temperature to prepare a 5 wt% plant active ingredient solution;
step 4, adding the 5 wt% of plant active ingredient solution prepared in the step 3 into the solution B in the step 22, and uniformly stirring at room temperature to obtain a solution C;
step 5, dropwise adding 1 wt% sodium tripolyphosphate solution into the solution C at the speed of 0.02mL/s, and stirring at the stirring speed of 500r/min for 60-80min at room temperature to form a nanocapsule dispersion liquid;
and 6, centrifuging the nano-capsule dispersion liquid obtained in the step 5 at 10000rpm for 20-30min, and then taking supernatant liquid to obtain the active agent through ultrasonic dispersion.
5. The method of claim 4, wherein the ultrasonic dispersion power of step S3 is 400w and the ultrasonic dispersion time is 15-20 min.
6. The method of claim 4 or 5, wherein the ultrasonic dispersion power of step 6 is 300w and the ultrasonic dispersion time is 10-12 min.
7. The method of claim 6, wherein step 6 is followed by the addition of the following steps: step 7, adding 40 wt% of sodium hydroxide solution and chloroacetic acid into the active agent, wherein the weight ratio of the nano sustained-release capsule, the 40 wt% of sodium hydroxide solution and the chloroacetic acid is 20: 100:1, reacting for 60-80min at 0-5 ℃ to prepare the carboxymethyl activating agent.
8. A LYOCELL fiber containing a plant active ingredient produced by the method of any one of claims 1-7.
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| CN114059186A (en) * | 2021-11-04 | 2022-02-18 | 青岛邦特生态纺织科技有限公司 | Ginger extract fiber and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114059186A (en) * | 2021-11-04 | 2022-02-18 | 青岛邦特生态纺织科技有限公司 | Ginger extract fiber and preparation method thereof |
| CN114059186B (en) * | 2021-11-04 | 2023-12-29 | 青岛邦特生态纺织科技有限公司 | Ginger extract fiber and preparation method thereof |
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