CN116555931A - Preparation method of antibacterial deodorizing regenerated cellulose fiber - Google Patents
Preparation method of antibacterial deodorizing regenerated cellulose fiber Download PDFInfo
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- CN116555931A CN116555931A CN202310660889.5A CN202310660889A CN116555931A CN 116555931 A CN116555931 A CN 116555931A CN 202310660889 A CN202310660889 A CN 202310660889A CN 116555931 A CN116555931 A CN 116555931A
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- regenerated cellulose
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- essential oil
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- oregano
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 42
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- 238000002156 mixing Methods 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 238000004061 bleaching Methods 0.000 claims description 10
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
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- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 5
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- 238000003756 stirring Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 5
- 229960001763 zinc sulfate Drugs 0.000 claims description 5
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- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- 239000004480 active ingredient Substances 0.000 claims description 4
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- 239000010902 straw Substances 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- 244000025254 Cannabis sativa Species 0.000 claims description 2
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 claims description 2
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 claims description 2
- 102000008186 Collagen Human genes 0.000 claims description 2
- 108010035532 Collagen Proteins 0.000 claims description 2
- 229920000875 Dissolving pulp Polymers 0.000 claims description 2
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- 239000001785 acacia senegal l. willd gum Substances 0.000 claims description 2
- 235000009120 camo Nutrition 0.000 claims description 2
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- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- 229940083575 sodium dodecyl sulfate Drugs 0.000 claims 1
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- 241001529744 Origanum Species 0.000 abstract description 15
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- 239000004753 textile Substances 0.000 abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
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- 230000036528 appetite Effects 0.000 description 2
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- 238000004332 deodorization Methods 0.000 description 2
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- 238000011156 evaluation Methods 0.000 description 2
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- 241000222122 Candida albicans Species 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 206010030113 Oedema Diseases 0.000 description 1
- 235000010677 Origanum vulgare Nutrition 0.000 description 1
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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
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a preparation method of antibacterial deodorizing regenerated cellulose fibers, and relates to the technical field of functional regenerated cellulose fibers. The cellulose adsorption resin is prepared by using cellulose fibers, is in a highly crosslinked porous network structure, has adsorption performance similar to that of active carbon, is prepared by using origanum essential oil, gelatin and acacia as raw materials, is used as a carrier, is used for adsorbing the origanum essential oil microcapsule, is mixed and dispersed with origanum extract, can stably exist in viscose, is uniformly dispersed, and is spun together. The regenerated cellulose fiber prepared by the invention has the effects of resisting bacteria and deodorizing, can be used for developing the application of origanum in the textile field, and improves the added value of textiles.
Description
Technical Field
The invention relates to the technical field of functional regenerated cellulose fibers, in particular to a preparation method of an antibacterial deodorizing regenerated cellulose fiber.
Background
Along with the progress of economic globalization, along with the desire of people for "returning to nature", the development and application of healthy, green and multifunctional textiles are more and more focused, and the "green, environment-friendly, healthy and comfortable" will extend through the whole textile industry. The regenerated cellulose fiber is taken from nature, the material source is rich and renewable, the regenerated cellulose fiber can be naturally biodegraded, the regenerated cellulose fiber is comfortable to wear, and the waste can be recycled without polluting the environment. Along with the enhancement of environmental awareness, the cellulose fabric becomes the first choice of consumers.
Oregano (Origano vulgare L.), also known as Origani, herba Moslae, herba Menthae, etc., the Labiatae Oregano perennial half shrubs or herbs. In China, the Chinese medicinal materials are mainly distributed in places such as Henan, jiangsu, zhejiang, jiangxi and Fujian. Oregano is pungent in taste, cool in nature, nontoxic, and capable of being used as a medicine by whole herb, and has the effects of clearing heat, relieving exterior syndrome, regulating qi, resolving dampness, inducing urination and reducing edema. The origanum vulgare whole herb can be used for extracting aromatic oil, can be used as a fragrance bud for being used as a medicine, and can also be used as a resource plant. The data of the United states department of agriculture, phytochemistry and plant species science, show that Oregano contains more than 30 antibacterial compounds, and has the effects of promoting urination, stimulating appetite, improving digestion, eliminating phlegm, resisting bacteria, and the like.
The adsorption resin is a highly crosslinked reticular, porous, ion exchange group-free, insoluble organic polymer granular material, has adsorption performance similar to that of activated carbon, and is widely applied. At the same time, the network structure and the high specific surface area make it have screening properties.
Therefore, the origanum extract and the cellulose adsorption resin are combined, on one hand, the application of origanum in the textile field is developed, the reasonable allocation of resources is realized, on the other hand, the added value of the textile is improved, and the requirements of consumers are met.
Disclosure of Invention
The invention aims to provide a preparation method of antibacterial deodorizing regenerated cellulose fibers, which aims to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme: the preparation method of the antibacterial deodorizing regenerated cellulose fiber comprises the following preparation steps:
(1) Dissolving cellulose fiber in distilled water, adding an initiator and a styrene monomer, treating in an ultrasonic oscillator with power of 1500W and oscillation frequency of 28kHz for 2 hours to obtain polymer gel, purifying, and drying to obtain cellulose adsorption resin;
(2) Mixing gelatin and Arabic gum according to the mass ratio of 0.6:1-1:1, dissolving in distilled water at 60 ℃ to prepare saturated solution, then dropwise adding the oregano essential oil mixed solution into the saturated solution, stirring for 3-4.5 hours in a water bath at 45 ℃ at 300r/min, cooling to room temperature, curing glutaraldehyde, washing with water, filtering, and vacuum drying to obtain oregano essential oil microcapsules;
(3) Placing cellulose adsorption resin and oregano essential oil microcapsule in water solution containing dispersing agent, fully adsorbing, and adding oregano extract to obtain composite additive solution;
(4) Mixing the viscose liquid and the composite additive solution, spinning through a coagulating bath, drawing the primary tows to obtain formed tows, and then cutting, desulfurizing, bleaching, oiling, washing and other refining baths and drying to obtain the antibacterial deodorizing regenerated cellulose fibers.
Further, the mass ratio of the cellulose fiber to distilled water in the step (1) is 1:10-1:20.
Further, the cellulose fiber in the step (1) is formed by mixing one or more of cotton fiber, ramie fiber, hemp fiber or straw fiber.
Further, the origanum essential oil mixed solution in the step (2) is prepared by mixing origanum essential oil and absolute ethyl alcohol according to the volume ratio of 1:1.
Further, the mass ratio of the cellulose adsorption resin, the oregano essential oil microcapsule and the oregano extract in the step (3) is 1:1.0:0.8-1:1.2:0.8.
Further, the dispersing agent in the step (3) is one or more of sodium dodecyl benzene sulfonate, sodium dodecyl sulfonate or sodium dodecyl sulfate.
Further, the proportion of the composite additive solution in the step (4) to the alpha cellulose content in the viscous collagen liquid is 10-18 wt% calculated according to the active ingredients.
Further, the coagulation bath of step (4): 65-122 g/L of sulfuric acid, 6.5-13.6 g/L of zinc sulfate and 273-345 g/L of sodium sulfate; the desulfurization bath: na (Na) 2 SO 3 2.0-7.2 g/L; the bleaching bath: h 2 O 2 2.2-4.5 g/L; the oil bath: 2.1 to 6.9g/L; the drying temperature is 112-125 ℃.
Further, the antibacterial deodorizing regenerated cellulose fiber contains 5-10% by weight of cellulose adsorption resin, 4-8% by weight of oregano extract and 8-10% by weight of oregano essential oil microcapsule.
Compared with the prior art, the invention has the following beneficial effects:
the invention utilizes cellulose to prepare the adsorption resin and then prepares the oregano essential oil microcapsule, and the oregano contains more than 30 antibacterial compounds, has the functions of promoting urination, promoting appetite, improving digestion, removing phlegm, resisting bacteria and the like, and is a natural antibacterial additive; adopting cellulose adsorption resin with stronger adsorptivity as a carrier to fully adsorb the origanum essential oil microcapsule aqueous solution and load more origanum essential oil microcapsules, then fully mixing the cellulose adsorption resin with the origanum extract aqueous solution, and carrying out wet spinning with viscose liquid to obtain the functional regenerated cellulose fiber with good antibacterial and deodorizing performances and lasting antibacterial function; tests prove that the antibacterial rate of the fiber to staphylococcus aureus is more than or equal to 95%, the antibacterial rate to escherichia coli is more than or equal to 90%, the antibacterial rate to candida albicans is up to 85.5%, and the deodorization rate of knitted fabrics prepared by the fiber is up to 80%; the functional regenerated cellulose fiber has good antibacterial performance, excellent wear performance and good textile processing performance, can be widely applied to the fields of bedding, clothing and medical supplies, and also develops the application of oregano in the textile field.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
(1) Dissolving cotton fibers in distilled water, wherein the mass ratio of the cotton fibers to the distilled water is 1:10, adding an initiator and a styrene monomer, treating for 2 hours in an ultrasonic oscillator with the power of 1500W and the oscillation frequency of 28kHz to obtain polymer gel, purifying and drying to obtain cellulose adsorption resin;
(2) Mixing gelatin and acacia in a mass ratio of 0.6:1, dissolving in distilled water at 60 ℃ to prepare a saturated solution, then dropwise adding the oregano essential oil mixed solution into the saturated solution, wherein the volume ratio of the oregano essential oil to absolute ethyl alcohol in the oregano essential oil mixed solution is 1:1, stirring in a water bath at 45 ℃ for 3 hours at 300r/min, cooling to room temperature, solidifying glutaraldehyde, washing with water, filtering, and vacuum drying to obtain oregano essential oil microcapsules;
(3) Placing cellulose adsorption resin and oregano essential oil microcapsule in an aqueous solution containing sodium dodecyl benzene sulfonate according to the mass ratio of 1:1, fully adsorbing, and adding oregano extract with the mass of 0.8 times that of the cellulose adsorption resin to prepare a composite additive solution;
(4) Adding a composite additive solution accounting for 10 weight percent of alpha cellulose in the viscose stock solution according to the calculation of active ingredients, spinning through a coagulating bath, drawing a primary tow to obtain a formed tow, and then cutting, desulfurizing, bleaching, oiling, washing and other scouring baths and drying to obtain the antibacterial deodorizing regenerated cellulose fiber with the thickness of 1.33dtex multiplied by 38 mm; the coagulation bath: 70g/L of sulfuric acid, 6.9g/L of zinc sulfate and 318g/L of sodium sulfate; the desulfurization bath: na (Na) 2 SO 3 2.5g/L; the bleaching bath: h 2 O 2 4.5g/L; the oil bath: 5.4g/L; the drying temperature is 115 ℃.
Example 2
(1) Dissolving ramie fibers in distilled water, wherein the mass ratio of the ramie fibers to the distilled water is 1:15, adding an initiator and a styrene monomer, treating for 2 hours in an ultrasonic oscillator with the power of 1500W and the oscillation frequency of 28kHz to obtain polymer gel, purifying and drying to obtain cellulose adsorption resin;
(2) Mixing gelatin and acacia in a mass ratio of 0.8:1, dissolving in distilled water at 60 ℃ to prepare a saturated solution, then dropwise adding the origanum essential oil mixed solution into the saturated solution, wherein the volume ratio of origanum essential oil to absolute ethyl alcohol in the origanum essential oil mixed solution is 1:1, stirring in a water bath at 45 ℃ for 3.7h at 300r/min, cooling to room temperature, curing glutaraldehyde, washing with water, filtering, and vacuum drying to obtain origanum essential oil microcapsules;
(3) Placing cellulose adsorption resin and oregano essential oil microcapsule in an aqueous solution containing sodium dodecyl sulfate according to the mass ratio of 1:1.1, fully adsorbing, and adding oregano extract with the mass of 0.8 times that of the cellulose adsorption resin to prepare a composite additive solution;
(4) Adding a compound additive solution accounting for 15wt% of alpha cellulose in the viscose stock solution according to the calculation of active ingredients, spinning through a coagulating bath, drawing a primary tow to obtain a formed tow, and then cutting, desulfurizing, bleaching, oiling, washing and other scouring baths and drying to obtain the antibacterial deodorizing regenerated cellulose fiber with the thickness of 1.67dtex multiplied by 38 mm; the coagulation bath: 81g/L of sulfuric acid, 7.7g/L of zinc sulfate and 323g/L of sodium sulfate; the desulfurization bath: na (Na) 2 SO 3 3.1g/L; the bleaching bath: h 2 O 2 3.9g/L; the oil bath: 5.0g/L; the drying temperature is 123 ℃.
Example 3
(1) Dissolving straw fibers in distilled water, wherein the mass ratio of the straw fibers to the distilled water is 1:20, adding an initiator and a styrene monomer, treating for 2 hours in an ultrasonic oscillator with the power of 1500W and the oscillation frequency of 28kHz to obtain polymer gel, purifying and drying to obtain cellulose adsorption resin;
(2) Mixing gelatin and acacia in a mass ratio of 1:1, dissolving in distilled water at 60 ℃ to prepare a saturated solution, then dropwise adding the oregano essential oil mixed solution into the saturated solution, wherein the volume ratio of the oregano essential oil to the absolute ethyl alcohol in the oregano essential oil mixed solution is 1:1, stirring in a water bath at 45 ℃ for 4.5 hours at 300r/min, cooling to room temperature, solidifying glutaraldehyde, washing with water, filtering, and vacuum drying to obtain oregano essential oil microcapsules;
(3) Placing cellulose adsorption resin and oregano essential oil microcapsule in an aqueous solution containing sodium dodecyl sulfate according to the mass ratio of 1:1.2, fully adsorbing, and adding oregano extract with the mass of 0.8 times that of the cellulose adsorption resin to prepare a composite additive solution;
(4) Adding alpha cellulose in the viscose stock solution according to the calculation of the active ingredientsSpinning the composite additive solution with the content of 18 weight percent through a coagulating bath, drawing a primary tow to obtain a formed tow, and then cutting, desulfurizing, bleaching, oiling, washing and other scouring baths and drying to obtain the antibacterial deodorizing regenerated cellulose fiber with the thickness of 2.22dtex multiplied by 56 mm; the coagulation bath: 94g/L of sulfuric acid, 6.9g/L of zinc sulfate and 308g/L of sodium sulfate; the desulfurization bath: na (Na) 2 SO 3 3.6g/L; the bleaching bath: h 2 O 2 4.8g/L; the oil bath: 5.4g/L; the drying temperature is 120 ℃.
Effect example
The results of the antibacterial property analysis of the antibacterial deodorizing regenerated cellulose fibers using examples 1 to 3 of the present invention are given in the following table 1; the following table 2 gives the results of analysis of deodorizing properties of the antibacterial deodorizing regenerated cellulose fibers according to examples 1 to 3 of the present invention.
Table 1 antibacterial property evaluation results of antibacterial deodorizing regenerated cellulose fibers of examples 1 to 3
Table 2 results of evaluation of deodorizing properties of antibacterial deodorizing regenerated cellulose fibers of examples 1 to 3
As can be seen from experimental data of the antibacterial rate and the odor reduction rate of the embodiment, the invention adopts the cellulose adsorption resin with stronger adsorptivity as a carrier, and the cellulose adsorption resin is a highly crosslinked net-shaped, porous, ion exchange group-free, insoluble organic polymer granular material, and has adsorption performance similar to that of activated carbon, so that the fiber deodorization effect is good, and the adsorption fixation of essential oil microcapsules is also facilitated; then, more oregano essential oil microcapsules are loaded, and meanwhile, the oregano extract is used for preparing a functional mixed solution, and the oregano contains more than 30 antibacterial compounds through wet spinning, so that the antibacterial effect is good, and the functional regenerated cellulose fiber prepared by the method is good in antibacterial and deodorizing performance and durable in antibacterial function.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (9)
1. The preparation method of the antibacterial deodorizing regenerated cellulose fiber is characterized by comprising the following preparation steps:
(1) Dissolving cellulose fiber in distilled water, adding an initiator and a styrene monomer, treating in an ultrasonic oscillator with power of 1500W and oscillation frequency of 28kHz for 2 hours to obtain polymer gel, purifying, and drying to obtain cellulose adsorption resin;
(2) Mixing gelatin and Arabic gum according to the mass ratio of 0.6:1-1:1, dissolving in distilled water at 60 ℃ to prepare saturated solution, then dropwise adding the oregano essential oil mixed solution into the saturated solution, stirring for 3-4.5 hours in a water bath at 45 ℃ at 300r/min, cooling to room temperature, curing glutaraldehyde, washing with water, filtering, and vacuum drying to obtain oregano essential oil microcapsules;
(3) Placing cellulose adsorption resin and oregano essential oil microcapsule in water solution containing dispersing agent, fully adsorbing, and adding oregano extract to obtain composite additive solution;
(4) Mixing the viscose liquid and the composite additive solution, spinning through a coagulating bath, drawing the primary tows to obtain formed tows, and then cutting, desulfurizing, bleaching, oiling, washing and other refining baths and drying to obtain the antibacterial deodorizing regenerated cellulose fibers.
2. The method for producing an antibacterial deodorizing regenerated cellulose fiber according to claim 1, wherein the mass ratio of the cellulose fiber in step (1) to distilled water is 1:10 to 1:20.
3. The method for producing an antibacterial deodorizing regenerated cellulose fiber according to claim 1, wherein the cellulose fiber in step (1) is composed of one or more of cotton fiber, ramie fiber, hemp fiber or straw fiber.
4. The method for preparing the antibacterial deodorizing regenerated cellulose fiber according to claim 1, wherein the oregano essential oil mixed solution in the step (2) is obtained by mixing oregano essential oil and absolute ethyl alcohol in a volume ratio of 1:1.
5. The method for preparing the antibacterial deodorizing regenerated cellulose fiber according to claim 1, wherein the mass ratio of the cellulose adsorption resin, the oregano essential oil microcapsule and the oregano extract in the step (3) is 1:1.0: 0.8-1:1.2: 0.8.
6. the method for producing an antibacterial deodorizing regenerated cellulose fiber according to claim 1, wherein the dispersant in step (3) is one or more of sodium dodecylbenzene sulfonate, sodium dodecylsulfonate or sodium dodecylsulfate.
7. The method for producing an antibacterial deodorizing regenerated cellulose fiber according to claim 1, wherein the composite additive solution in step (4) is added in a proportion of 10 to 18% by weight based on the active ingredient, based on the content of alpha cellulose in the viscous collagen liquid.
8. The method for producing an antibacterial deodorizing regenerated cellulose fiber according to claim 1, wherein the coagulation bath of step (4) is: 65-122 g/L of sulfuric acid, 6.5-13.6 g/L of zinc sulfate and 273-345 g/L of sodium sulfate; the desulfurization bath: na (Na) 2 SO 3 2.0～7.2g/L; the bleaching bath: h 2 O 2 2.2-4.5 g/L; the oil bath: 2.1 to 6.9g/L; the drying temperature is 112-125 ℃.
9. The method for preparing the antibacterial deodorizing regenerated cellulose fiber according to claim 1, wherein the antibacterial deodorizing regenerated cellulose fiber contains 5-10% by weight of cellulose adsorption resin, 4-8% by weight of oregano extract and 8-10% by weight of oregano essential oil microcapsule.
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