CN113512886A - Essential oil-loaded cellulose fiber and preparation method thereof - Google Patents

Essential oil-loaded cellulose fiber and preparation method thereof Download PDF

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Publication number
CN113512886A
CN113512886A CN202010273486.1A CN202010273486A CN113512886A CN 113512886 A CN113512886 A CN 113512886A CN 202010273486 A CN202010273486 A CN 202010273486A CN 113512886 A CN113512886 A CN 113512886A
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essential oil
cellulose
solution
aqueous solution
loaded
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王闻宇
曾原
钱晓明
金欣
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China Merchants Health Industry Qichun Co ltd
Tianjin Polytechnic University
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China Merchants Health Industry Qichun Co ltd
Tianjin Polytechnic University
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M23/00Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
    • D06M23/02Processes in which the treating agent is releasably affixed or incorporated into a dispensing means
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03Polysaccharides or derivatives thereof
    • D06M15/05Cellulose or derivatives thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic

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  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention relates to the technical field of functional fibers, and particularly relates to essential oil-loaded cellulose fibers and a preparation method thereof. The preparation method of the essential oil-loaded cellulose fiber provided by the invention comprises the following steps: mixing the essential oil solution and the embedding agent saturated aqueous solution to obtain an embedded essential oil dispersion liquid; the embedding agent in the embedding agent saturated aqueous solution is cyclodextrin or cyclodextrin derivatives; dissolving cellulose pulp in an N-methylmorpholine-N-oxide aqueous solution to obtain a cellulose solution; dropwise adding the embedding essential oil dispersion liquid into the cellulose solution to obtain a coating liquid; and coating the coating liquid on the surface of the cellulose fiber, and curing in a coagulating bath to obtain the essential oil-loaded cellulose fiber. The essential oil loaded cellulose fiber prepared by the invention has a slow release effect and can ensure the continuous exertion of the drug effect of the essential oil; in addition, the essential oil can be firmly fixed on the surface of the cellulose fiber by utilizing the action of the embedding agent and the cellulose, and the durability is good.

Description

Essential oil-loaded cellulose fiber and preparation method thereof
Technical Field
The invention relates to the technical field of functional fibers, and particularly relates to essential oil-loaded cellulose fibers and a preparation method thereof.
Background
The cellulose fiber belongs to biomass regenerated fiber, is comfortable to wear, beautiful in dyeing, soft, plump and smooth in hand feeling and is popular with consumers, and meanwhile, the cellulose fiber belongs to the biomass regenerated fiber, is prepared from natural plants, can be biodegraded, is wide in source and has a very large development space for increasingly exhausted petroleum resources.
Because of the characteristics of the cellulose fiber such as non-toxicity, comfortable wearing, skin friendliness and the like, textile fabrics containing the cellulose fiber component are more and more popular with people, people also hope that the biomass fiber can provide functions such as antibiosis, health care, sterilization and the like while improving the comfort,
the existing cellulose fiber treatment methods mainly comprise the following steps: (1) the surface coating method is that the functional agent and the coating agent are mixed together and coated on the surface of the fiber, and the functional agent in the cellulose fiber obtained by the treatment method is easy to fall off and has no slow release function; (2) the mixed processing method is usually to directly add the functional agent into the fiber for blending, the processing method has good durability, but the loss of the effective component of the functional agent is large in the processing process; (3) the finishing method after dyeing and finishing is generally to add antibacterial finishing in the fiber dyeing process, and utilize the antibacterial agent contained in some dyes to carry out dyeing finishing, but the content of the antibacterial agent added in the method is less, and the expected effect is difficult to achieve.
Disclosure of Invention
The invention aims to provide a preparation method of essential oil loaded cellulose fibers, and the essential oil loaded cellulose fibers prepared by the invention have a slow release effect and can ensure the continuous exertion of the drug effect of essential oil; in addition, the essential oil can be firmly fixed on the surface of the cellulose fiber by utilizing the action of the embedding agent and the cellulose, and the durability is good.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of essential oil-loaded cellulose fibers, which comprises the following steps:
(1) mixing the essential oil solution and the embedding agent saturated aqueous solution to obtain an embedded essential oil dispersion liquid; the embedding agent in the embedding agent saturated aqueous solution is cyclodextrin or cyclodextrin derivatives;
(2) dissolving cellulose pulp in an N-methylmorpholine-N-oxide aqueous solution to obtain a cellulose solution;
(3) dropwise adding the embedding essential oil dispersion liquid into the cellulose solution to obtain a coating liquid;
(4) coating the coating liquid on the surface of cellulose fiber, and placing the cellulose fiber in a coagulating bath for solidification to obtain essential oil-loaded cellulose fiber;
the steps (1) and (2) are not limited in chronological order.
Preferably, the temperature of the mixing in the step (1) is 50-90 ℃; the mixing mode is as follows: and dropwise adding the essential oil solution into the embedding agent saturated aqueous solution.
Preferably, the mass ratio of the essential oil in the essential oil solution to the embedding agent in the embedding agent saturated water solution is (5-15): 100.
preferably, the cellulose content in the cellulose solution of step (2) is 8-15 wt.%.
Preferably, the dropping speed in the step (3) is 30-90 drops/min.
Preferably, the mass ratio of the embedding agent to the cellulose in the coating liquid is (1-5): 100.
preferably, the coagulating bath in step (4) is water or an aqueous solution of N-methylmorpholine-N-oxide.
The invention provides essential oil-loaded cellulose fibers prepared by the preparation method in the technical scheme, which comprise cellulose fibers and cellulose membranes loaded on the surfaces of the cellulose fibers; the cellulose membrane is internally wrapped with essential oil embedded by an embedding medium.
Preferably, the loading amount of the essential oil is 0.05-0.5 wt.%.
The invention provides a preparation method of essential oil-loaded cellulose fibers, which comprises the following steps: (1) mixing the essential oil solution and the embedding agent saturated aqueous solution to obtain an embedded essential oil dispersion liquid; the embedding agent in the embedding agent saturated aqueous solution is cyclodextrin or cyclodextrin derivatives; (2) dissolving cellulose pulp in an N-methylmorpholine-N-oxide aqueous solution to obtain a cellulose solution; (3) dropwise adding the embedding essential oil dispersion liquid into the cellulose solution to obtain a coating liquid; (4) coating the coating liquid on the surface of cellulose fiber, and placing the cellulose fiber in a coagulating bath for solidification to obtain essential oil-loaded cellulose fiber; the steps (1) and (2) are not limited in chronological order. In the invention, the cyclodextrin has a unique molecular structure of a hydrophobic center and a hydrophilic surface, and the essential oil is embedded by adopting the cyclodextrin or the cyclodextrin derivative, so that the essential oil can be embedded in the molecular center of the cyclodextrin or the cyclodextrin derivative, and the essential oil is protected and slowly released; by mixing the embedding essential oil dispersion liquid and the cellulose solution, the embedding essential oil dispersion liquid can be uniformly dispersed in the cellulose solution; when cellulose is solidified in a coagulating bath, a cellulose membrane with higher density can be formed on the surface of cellulose fiber, so that essential oil embedded by an embedding agent is fixed in the cellulose membrane and is completely embedded in the cellulose membrane, and because the components of cellulose pulp and the cellulose fiber are the same, the binding force of the essential oil and the cellulose fiber can be improved, the controlled release effect of the essential oil can be improved, and then the essential oil-loaded cellulose fiber with a slow release function and excellent durability can be obtained.
Drawings
FIG. 1 is an SEM image of essential oil-loaded cellulose fibers prepared in example 1;
FIG. 2 is an SEM image of cellulose fibers prepared in comparative example 1;
FIG. 3 is an SEM image of essential oil-loaded cellulose fibers prepared in example 1 after being washed 100 times with water;
FIG. 4 is an SEM photograph of the cellulose fiber prepared in comparative example 1 after being washed 100 times with water;
FIG. 5 is a graph of the strength of the products prepared in comparative example 1 and examples 1 to 4;
FIG. 6 is a modulus plot of the products prepared in comparative example 1 and examples 1-4;
FIG. 7 is a graph of the cumulative release rate of essential oil from essential oil-loaded cellulose fibers prepared in examples 5-8.
Detailed Description
The invention provides a preparation method of essential oil-loaded cellulose fibers, which comprises the following steps:
(1) mixing the essential oil solution and the embedding agent saturated aqueous solution to obtain an embedded essential oil dispersion liquid; the embedding agent in the embedding agent saturated aqueous solution is cyclodextrin or cyclodextrin derivatives;
(2) dissolving cellulose pulp in an N-methylmorpholine-N-oxide aqueous solution to obtain a cellulose solution;
(3) dropwise adding the embedding essential oil dispersion liquid into the cellulose solution to obtain a coating liquid;
(4) coating the coating liquid on the surface of cellulose fiber, and placing the cellulose fiber in a coagulating bath for solidification to obtain essential oil-loaded cellulose fiber;
the steps (1) and (2) are not limited in chronological order.
The essential oil solution and the embedding agent saturated aqueous solution are mixed to obtain the embedded essential oil dispersion liquid. In the present invention, the essential oil in the essential oil solution is preferably an aromatic essential oil, and is particularly preferably wormwood essential oil or lavender essential oil. The invention adopts the essential oil with the effects of calming the nerves and resisting bacteria, and can endow the cellulose fiber with the effects of resisting bacteria and calming the nerves. In the invention, the effective content of the essential oil is preferably 0.06-0.2%, and more preferably 0.07-0.1%. In the present invention, the solvent of the essential oil solution is preferably absolute ethyl alcohol. In the invention, the mass content of the essential oil in the essential oil solution is preferably 40-60%, more preferably 45-55%, and most preferably 50%.
In the invention, the embedding agent in the embedding agent saturated aqueous solution is cyclodextrin or cyclodextrin derivative, preferably water-soluble cyclodextrin or cyclodextrin derivative; the cyclodextrin is preferably alpha-cyclodextrin, beta-cyclodextrin or gamma-cyclodextrin; the cyclodextrin derivative is preferably hydroxypropyl-beta-cyclodextrin. In the invention, the cyclodextrin is a starch oligomer processed by enzymolysis and purification of starch, a plurality of pyranose units are connected by alpha glycosidic bonds to form a large circular structure of hydrophilic groups outside a middle hydrophobic group, and the cyclodextrin can be used as an embedding agent for embedding essential oil by virtue of the unique hydrophobic center and hydrophilic surface structure to play a role of slow release.
In the invention, the temperature of the embedding agent saturated aqueous solution is preferably 50-90 ℃, and more preferably 60-85 ℃. In the invention, the mass ratio of the essential oil in the essential oil solution to the embedding agent in the embedding agent saturated water solution is preferably (5-15): 100, more preferably (6-11): 100, more preferably (7-10): 100.
in the present invention, the mixing is preferably performed in the following manner: and dropwise adding the essential oil solution into the embedding agent saturated aqueous solution. In the invention, the dripping speed is preferably 30-90 drops/min, and more preferably 40-60 drops/min; and in the dropping process, keeping the temperature of the embedding agent saturated aqueous solution at 50-90 ℃, and more preferably at 85 ℃.
In the mixing process of the essential oil solution and the embedding agent saturated aqueous solution, white precipitate is formed, and the embedded essential oil dispersion liquid with the essential oil embedded in the embedding agent is obtained.
The cellulose pulp is dissolved in an N-methylmorpholine-N-oxide aqueous solution to obtain a cellulose solution. In the present invention, the cellulose pulp is preferably a lignocellulose pulp, a bamboo cellulose pulp or a ramie cellulose pulp; the cellulose pulp preferably has the same composition as the cellulose fibers. In the present invention, the water content of the aqueous solution of N-methylmorpholine-N-oxide is preferably less than 13.3%, more preferably 5 to 8%. The invention can prevent cellulose from being separated out in advance by controlling the water content of the N-methylmorpholine-N-oxide aqueous solution in the range. In the invention, the dissolving temperature of the cellulose pulp in the N-methylmorpholine-N-oxide aqueous solution is preferably 60-90 ℃, and more preferably 70-85 ℃.
In the invention, the mass content of the cellulose in the cellulose solution is preferably 8-15 wt.%, and more preferably 10-13 wt.%.
After the embedded essential oil dispersion liquid and the cellulose solution are obtained, the embedded essential oil dispersion liquid is dripped into the cellulose solution to obtain the coating liquid. In the invention, the mass ratio of the embedding agent to the cellulose is preferably (1-5): 100, more preferably (2-4): 100. in the invention, the dripping speed is preferably 30-90 drops/min, more preferably 50-60 drops/min, and the dripping method is favorable for improving the uniformity of the coating liquid.
After the coating liquid is obtained, the coating liquid is coated on the surface of the cellulose fiber and is placed in a coagulating bath for solidification, and the essential oil-loaded cellulose fiber is obtained. In the present invention, the coating is preferably performed by dipping, spraying or spin coating.
In the present invention, the coagulation bath is preferably water or an aqueous solution of N-methylmorpholine-N-oxide; the water is preferably pure water. In the present invention, the mass content of N-methylmorpholine-N-oxide in the aqueous solution of N-methylmorpholine-N-oxide is preferably 85% or more, more preferably 90%. According to the invention, the content of the N-methylmorpholine-N-oxide can influence the pore arrangement of the formed cellulose membrane, and the density of the cellulose membrane can be improved by controlling the content of the N-methylmorpholine-N-oxide within the range, so that the slow release effect of the essential oil can be improved.
In the invention, the curing temperature is preferably 20-60 ℃, and more preferably 25-50 ℃. In the solidification process, the cellulose fiber coated with the coating liquid is soaked in the coagulating bath, so that N-methylmorpholine-N-oxide (NMMO) in the cellulose solution can be replaced, the cellulose in the coating liquid is coagulated in water to form a compact cellulose film on the surface of the cellulose fiber, and the essential oil embedded by cyclodextrin is fixed in the cellulose film and is completely embedded in the cellulose film and is not easy to fall off.
In a specific embodiment of the present invention, after the curing, the fiber obtained by curing is preferably dried to obtain the essential oil-loaded cellulose fiber. In the invention, the drying temperature is preferably 40-80 ℃, and more preferably 60-70 ℃; the drying time is preferably 10-30 min, and more preferably 20-25 min.
The invention provides essential oil-loaded cellulose fibers prepared by the preparation method in the technical scheme, which comprise cellulose fibers and cellulose films loaded on the surfaces of the cellulose fibers; the cellulose membrane is internally wrapped with essential oil embedded by an embedding agent. In the invention, the loading amount of the essential oil is preferably 0.05-0.5 wt.%, and more preferably 0.08-0.3 wt.%. In the invention, the surface of the essential oil-loaded cellulose fiber is uniform micropores.
The essential oil-loaded cellulose fiber provided by the invention has good slow release performance, does not influence the strength of the cellulose fiber in the preparation process, has good use durability and wide application range, and is suitable for industrial production.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing a saturated aqueous solution of beta-cyclodextrin at 85 ℃; dissolving wormwood essential oil accounting for 10 wt.% of the mass of the beta-cyclodextrin in absolute ethyl alcohol with the same amount to obtain an essential oil solution; dropwise adding the essential oil solution into the beta-cyclodextrin saturated aqueous solution at 85 ℃ (the dropwise adding speed is 60 drops/min), forming white precipitate to obtain embedded essential oil dispersion, and keeping the temperature (85 ℃) for later use;
putting an NMMO aqueous solution with the water content of 6% into a water bath kettle at 85 ℃, then adding lignocellulose pulp, and obtaining a cellulose solution with the cellulose content of 15 wt.% after the cellulose pulp is completely dissolved;
dropwise adding the embedding essential oil dispersion liquid into the cellulose solution (the dropwise adding speed is 50 drops/min) to obtain a coating liquid; wherein, the content of the beta-cyclodextrin is 5 percent of the content of the cellulose; (ii) a
Uniformly coating the coating liquid on the surface of wood fiber, soaking in pure water, replacing NMMO, taking out the fiber, and drying at 50 ℃ for 20min to obtain the essential oil-loaded cellulose fiber.
Example 2
Preparing a saturated aqueous solution of gamma-cyclodextrin at 85 ℃; dissolving wormwood essential oil accounting for 8 wt.% of the mass of the gamma-cyclodextrin in absolute ethyl alcohol with the same amount to obtain an essential oil solution; dropwise adding the essential oil solution into the gamma-cyclodextrin saturated aqueous solution at 85 ℃ (the dropwise adding speed is 40 drops/min), forming white precipitate to obtain embedded essential oil dispersion, and keeping the temperature (85 ℃) for later use;
putting an NMMO aqueous solution with the water content of 8% into a water bath kettle at 85 ℃, then adding bamboo fiber pulp, and obtaining a cellulose solution with the cellulose content of 13 wt.% after the cellulose pulp is completely dissolved;
dropwise adding the embedding essential oil dispersion liquid into the cellulose solution (the dropwise adding speed is 50 drops/min) to obtain a coating liquid; wherein, the content of the gamma-cyclodextrin is 2 percent of the content of the cellulose; the cellulose content in the coating liquid was 10 wt.%;
and uniformly coating the coating liquid on the surface of the bamboo fiber, soaking in pure water, replacing NMMO, taking out the fiber, and drying at 30 ℃ for 30min to obtain the essential oil-loaded cellulose fiber.
Example 3
Preparing a saturated aqueous solution of beta-cyclodextrin at 85 ℃; dissolving lavender essential oil accounting for 10 wt.% of the mass of the beta-cyclodextrin into the same amount of absolute ethyl alcohol to obtain an essential oil solution; dropwise adding the essential oil solution into the beta-cyclodextrin saturated aqueous solution at 85 ℃ (the dropwise adding speed is 70 drops/min), forming white precipitate to obtain embedded essential oil dispersion, and keeping the temperature (85 ℃) for later use;
putting an NMMO aqueous solution with the water content of 10% into a water bath kettle at 85 ℃, then adding lignocellulose pulp, and obtaining a cellulose solution with the cellulose content of 13 wt.% after the cellulose pulp is completely dissolved;
dropwise adding the embedding essential oil dispersion liquid into the cellulose solution (the dropwise adding speed is 60 drops/min) to obtain a coating liquid; wherein the content of beta-cyclodextrin is 1 percent of the content of cellulose; the cellulose content in the coating liquid was 20 wt.%;
uniformly coating the coating liquid on the surface of the Lyocell fiber, soaking in pure water, replacing NMMO, taking out the fiber, and drying at 30 ℃ for 25min to obtain the essential oil-loaded cellulose fiber.
Example 4
Preparing a saturated aqueous solution of beta-cyclodextrin at 85 ℃; dissolving aromatic essential oil accounting for 10 wt.% of the mass of the beta-cyclodextrin in absolute ethyl alcohol with the same amount to obtain an essential oil solution; dropwise adding the essential oil solution into the beta-cyclodextrin saturated aqueous solution at 85 ℃ (the dropwise adding speed is 60 drops/min), forming white precipitate to obtain embedded essential oil dispersion, and keeping the temperature (85 ℃) for later use;
putting an NMMO aqueous solution with the water content of 5% into a water bath kettle at 85 ℃, then adding ramie cellulose pulp, and obtaining a cellulose solution with the cellulose content of 13 wt.% after the cellulose pulp is completely dissolved; cellulose content in the coating liquid was 5 wt.%;
dropwise adding the embedding essential oil dispersion liquid into the cellulose solution (the dropwise adding speed is 40 drops/min) to obtain a coating liquid; wherein the content of beta-cyclodextrin is 1 percent of the content of cellulose;
and uniformly coating the coating liquid on the surface of ramie fibers, soaking in pure water, replacing NMMO, taking out the fibers, and drying at 40 ℃ for 20min to obtain the essential oil-loaded cellulose fibers.
Example 5
The preparation process was substantially the same as in example 1 except that the beta-cyclodextrin content was 1% of the cellulose content.
Example 6
The preparation process was substantially the same as in example 1 except that the beta-cyclodextrin content was 2% of the cellulose content.
Example 7
The preparation process was substantially the same as in example 1 except that the beta-cyclodextrin content was 3% of the cellulose content.
Example 8
The preparation process was substantially the same as in example 1 except that the beta-cyclodextrin content was 4% of the cellulose content.
Comparative example 1
Preparing a saturated aqueous solution of beta-cyclodextrin at 85 ℃; dissolving wormwood essential oil accounting for 10 wt.% of the mass of the beta-cyclodextrin in absolute ethyl alcohol with the same amount to obtain an essential oil solution; dropwise adding the essential oil solution (the dropwise adding speed is 60 drops/min) into the beta-cyclodextrin saturated aqueous solution at 85 ℃ to form white precipitate to obtain embedded essential oil dispersion, and keeping the temperature for later use;
adding the embedding essential oil dispersion liquid into a polyacrylic acid adhesive (40% aqueous solution) to obtain a coating liquid;
and coating the coating liquid on the surface of the wood fiber, and drying for 5min at the temperature of 80 ℃ to obtain the coated fiber.
Test example 1
An SEM image of the essential oil-loaded cellulose fibers prepared in example 1 is shown in fig. 1; the SEM image of the coated fiber prepared in comparative example 1 is shown in fig. 2. As can be seen from the figures 1-2, because the coating of the fiber prepared by the invention has a certain amount of solvent double diffusion in the curing process, the surface of the prepared essential oil loaded cellulose fiber is uniform micropores and also plays a role in the sustained and controlled release of essential oil; in the comparative example 1, the surface of the prepared coating fiber is compact by adopting the traditional coating method, and in the curing process, due to inconsistent extension and retraction, the surface is uneven, so that the hand feeling and the appearance of the fiber are poor.
Test example 2
After washing the essential oil-loaded cellulose fibers prepared in example 1 with water for 100 times, the SEM image is shown in fig. 3; the cellulose fiber prepared in comparative example 1 was washed with water 100 times, and the SEM image is shown in fig. 4. As can be seen from FIGS. 3 to 4, the preparation method provided by the invention can improve the service durability of the cellulose fiber.
Test example 3
The strength of the products prepared in comparative example 1 and examples 1 to 4 is shown in fig. 5, and the modulus of the products is shown in fig. 6. As can be seen from FIGS. 5 to 6, the method provided by the invention can improve the mechanical properties of the fibers.
Test example 4
The accumulative release rate of the essential oil loaded with the essential oil cellulose fibers prepared in examples 5-8 is shown in fig. 7, and it can be seen from fig. 7 that the controlled release capacity of the fibers to the essential oil is improved along with the increase of the content of cyclodextrin, and the drug can still be controlled within 60% in 160 hours, which shows that the controlled release effect of the preparation method of the invention to the essential oil is remarkable.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (9)

1. A preparation method of essential oil-loaded cellulose fibers comprises the following steps:
(1) mixing the essential oil solution and the embedding agent saturated aqueous solution to obtain an embedded essential oil dispersion liquid; the embedding agent in the embedding agent saturated aqueous solution is cyclodextrin or cyclodextrin derivatives;
(2) dissolving cellulose pulp in an N-methylmorpholine-N-oxide aqueous solution to obtain a cellulose solution;
(3) dropwise adding the embedding essential oil dispersion liquid into the cellulose solution to obtain a coating liquid;
(4) coating the coating liquid on the surface of cellulose fiber, and placing the cellulose fiber in a coagulating bath for solidification to obtain essential oil-loaded cellulose fiber;
the steps (1) and (2) are not limited in chronological order.
2. The method according to claim 1, wherein the temperature of the mixing in the step (1) is 50 to 90 ℃; the mixing mode is as follows: and dropwise adding the essential oil solution into the embedding agent saturated aqueous solution.
3. The preparation method according to claim 1 or 2, wherein the mass ratio of the essential oil in the essential oil solution to the embedding agent in the embedding agent saturated aqueous solution is (5-15): 100.
4. the method according to claim 1, wherein the cellulose content in the cellulose solution of step (2) is 8 to 15 wt.%.
5. The method according to claim 1, wherein the dropping speed in the step (3) is 30 to 90 drops/min.
6. The preparation method according to claim 1 or 5, wherein the mass ratio of the embedding agent to the cellulose in the coating liquid is (1-5): 100.
7. the method according to claim 1, wherein the coagulation bath in the step (4) is water or an aqueous solution of N-methylmorpholine-N-oxide.
8. Essential oil-loaded cellulose fibers prepared by the preparation method according to any one of claims 1 to 7, comprising cellulose fibers and a cellulose film loaded on the surfaces of the cellulose fibers; the cellulose membrane is internally wrapped with essential oil embedded by an embedding medium.
9. Essential oil loaded cellulose fibers according to claim 8, characterized in that the loading of the essential oil is 0.05 to 0.5 wt.%.
CN202010273486.1A 2020-04-09 2020-04-09 Essential oil-loaded cellulose fiber and preparation method thereof Pending CN113512886A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114224760A (en) * 2021-12-06 2022-03-25 北京美科兴业生物科技有限公司 Stable bacteriostatic composition and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996037653A1 (en) * 1995-05-22 1996-11-28 Akzo Nobel N.V. Shaped bodies coated, impregnated or covered with a cellulosic composition
JP2002065839A (en) * 2000-08-31 2002-03-05 Risoo Erudesu:Kk CELLULOSE SYSTEM FIBER WEB MATERIAL FOR HEALTH-SANITARY MEDICAL CARE HAVING MONOCHLOROTRIAZINYL-beta-CYCLODEXTRIN MATINGLY EMBLACING DRUGS, ETC., BY COVALENT BOND
CN103422339A (en) * 2013-08-23 2013-12-04 华南理工大学 Method for preparing antibacterial functional cellulosic fibers
CN107354738A (en) * 2017-09-04 2017-11-17 西南大学 Chitosan/cotton antibacterial composite fabric is prepared with NMMO

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996037653A1 (en) * 1995-05-22 1996-11-28 Akzo Nobel N.V. Shaped bodies coated, impregnated or covered with a cellulosic composition
JP2002065839A (en) * 2000-08-31 2002-03-05 Risoo Erudesu:Kk CELLULOSE SYSTEM FIBER WEB MATERIAL FOR HEALTH-SANITARY MEDICAL CARE HAVING MONOCHLOROTRIAZINYL-beta-CYCLODEXTRIN MATINGLY EMBLACING DRUGS, ETC., BY COVALENT BOND
CN103422339A (en) * 2013-08-23 2013-12-04 华南理工大学 Method for preparing antibacterial functional cellulosic fibers
CN107354738A (en) * 2017-09-04 2017-11-17 西南大学 Chitosan/cotton antibacterial composite fabric is prepared with NMMO

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
周春禾等: "尤加利精油制备微胶囊抗菌纤维素薄膜", 《包装工程》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114224760A (en) * 2021-12-06 2022-03-25 北京美科兴业生物科技有限公司 Stable bacteriostatic composition and preparation method and application thereof

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