CN115679681A - Preparation method of modified nano ZnO antibacterial cellulose fiber and fabric - Google Patents
Preparation method of modified nano ZnO antibacterial cellulose fiber and fabric Download PDFInfo
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- CN115679681A CN115679681A CN202211437572.7A CN202211437572A CN115679681A CN 115679681 A CN115679681 A CN 115679681A CN 202211437572 A CN202211437572 A CN 202211437572A CN 115679681 A CN115679681 A CN 115679681A
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- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 42
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 29
- 239000004744 fabric Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000002791 soaking Methods 0.000 claims abstract description 12
- 229920000642 polymer Polymers 0.000 claims abstract description 11
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 7
- 239000011701 zinc Substances 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 3
- 239000003381 stabilizer Substances 0.000 claims abstract description 3
- 229920000742 Cotton Polymers 0.000 claims description 11
- 239000000835 fiber Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- 229920000297 Rayon Polymers 0.000 claims description 9
- -1 modal Polymers 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 4
- 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
- 239000004593 Epoxy Substances 0.000 claims description 2
- 229920000433 Lyocell Polymers 0.000 claims description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 2
- 150000001348 alkyl chlorides Chemical class 0.000 claims description 2
- 235000009120 camo Nutrition 0.000 claims description 2
- 150000001767 cationic compounds Chemical class 0.000 claims description 2
- 235000005607 chanvre indien Nutrition 0.000 claims description 2
- 239000011487 hemp Substances 0.000 claims description 2
- 150000003335 secondary amines Chemical class 0.000 claims description 2
- 150000003512 tertiary amines Chemical class 0.000 claims description 2
- 239000004246 zinc acetate Substances 0.000 claims description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 2
- 229960001763 zinc sulfate Drugs 0.000 claims description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 2
- 241000588724 Escherichia coli Species 0.000 abstract description 3
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000004745 nonwoven fabric Substances 0.000 description 6
- 230000003385 bacteriostatic effect Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000003223 protective agent Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 1
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 description 1
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 description 1
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 229940043237 diethanolamine Drugs 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920000587 hyperbranched polymer Polymers 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229940014800 succinic anhydride Drugs 0.000 description 1
- 229960001124 trientine Drugs 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
- 230000003253 viricidal effect Effects 0.000 description 1
Images
Classifications
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- 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
Abstract
The invention relates to the technical field of medical antibacterial materials, in particular to a modified nano ZnO antibacterial cellulose fiber and a preparation method of fabricThe preparation method comprises the following steps: step 1, pretreating cellulose fibers; step 2, soaking the cellulose fiber or the fabric modified by polycation into Zn 2+ Adding alkali liquor into zinc ion aqueous solution with concentration of 40-400mg/L, controlling pH value to 9-12, and selecting electronegative carboxyl or hydroxyl high polymer as stabilizer; and 3, treating the impregnated cellulose fiber or fabric by using an ultrasonic emitter, wherein the ultrasonic frequency is 20-60kHz, and the ultrasonic time is 5-10min. The preparation method is simple, and the nano ZnO is easily combined with the cellulose fiber and can be uniformly dispersed on the cellulose fiber; the prepared nano ZnO loaded cellulose fiber is not easy to harden, has good antibacterial property, and has the antibacterial rate of over 99 percent on escherichia coli and staphylococcus aureus.
Description
Technical Field
The invention relates to the technical field of medical antibacterial materials, in particular to a preparation method of modified nano ZnO antibacterial cellulose fibers and fabrics.
Background
Cellulosic fiber products are widely used in apparel, bedding, bath products, and a variety of industrial applications. Cellulose fiber belongs to biomass, has good hydrophilicity and biocompatibility, and is particularly easy to attach and propagate bacteria. With the increase of health awareness of consumers, there is an increasing demand for antibacterial and virucidal textiles, which are also required to have excellent durability. For many years, the durable antibacterial properties of cellulose fibers have been a hot spot in international and domestic market demands due to the wide application of cellulose products in daily life.
Nano ZnO is a multifunctional inorganic material currently with wide application prospects. Because the nano ZnO particles are very small, the specific surface area of the nano ZnO particles is very large, the surface molecular arrangement, the electronic structure and the crystal structure are changed, and the nano ZnO particles have a surface effect, a small-size effect, a quantum size effect, a macroscopic quantum tunneling effect and the like. Therefore, the nano ZnO has a series of excellent physical, chemical, surface and interface properties, and has special performance and application which are incomparable with common ZnO in the aspects of magnetism, light, electricity, catalysis and the like. The combination of the cellulose fiber and the nano ZnO can simultaneously have the functions of adsorption and bacteriostasis, thus overcoming the disadvantage that the cellulose fiber can not inhibit bacteria and expanding the application range of the cellulose.
The literature, experimental research on microwave in-situ generation of nano ZnO finished cotton fabric, textile guide, 2013 and 09, reports a method for preparing supported nano ZnO by microwaves, cotton fabric is required to be sealed in a microwave oven, the possibility of mass production is limited, and the cotton adsorption effect of a protective agent is weak, so that the fastness is low. In the patent of a preparation method of a ZnO textile fabric composite material with antibacterial property, CN104775298A prepares a nano ZnO loaded fabric, the invention does not use a necessary protective agent, can be carried out under the assistance of microwave and ultrasonic wave, and has the problem of poor fastness. At present, no document reports a method for preparing nano ZnO loaded cotton fabric by ultrasonic energy reaction.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a preparation method of a modified nano ZnO antibacterial cellulose fiber and a fabric, which can endow cellulose with an antibacterial function.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of modified nano ZnO antibacterial cellulose fiber and fabric comprises the following steps:
step 1, pretreating cellulose fibers; soaking cellulose fiber or fabric into polycation solution at a bath ratio of 1;
step 2, soaking the cellulose fiber or the fabric modified by polycation into Zn 2+ Adding alkali liquor into zinc ion aqueous solution with concentration of 40-400mg/L, controlling pH value to 9-12, and selecting electronegative carboxyl or hydroxyl high polymer as stabilizer;
and 3, treating the impregnated cellulose fiber or fabric by using an ultrasonic emitter, wherein the ultrasonic frequency is 20-60kHz, and the ultrasonic time is 5-10min.
Preferably, in step 1, the cellulosic fibres comprise cotton, viscose, modal, lyocell or hemp fibres.
Preferably, in step 1, the polycation is a cationic compound polymerized by epoxy chloroalkane, secondary amine and tertiary amine.
Preferably, in step 2, the aqueous solution of zinc ions is an aqueous solution of zinc nitrate, zinc sulfate or zinc acetate.
Preferably, in step 2, the electronegative polymer is a terminal carboxyl polymer having an isoelectric point of 6 or less, or a terminal carboxyl polymer.
Compared with the prior art, the invention has the following beneficial effects:
the loaded nano ZnO cellulose fiber and fabric prepared by the invention are not easy to harden, have good fluffiness and good nano ZnO dispersibility, and the prepared fiber has good antibacterial property, and the antibacterial rate of the fiber on escherichia coli and staphylococcus aureus can reach more than 99%.
Drawings
FIG. 1 is an electron microscope image of a cotton fiber loaded with ZnO in example 1 of the present invention;
FIG. 2 is an electron microscope image of ZnO loaded viscose fibers in example 2 of the present invention;
FIG. 3 is a bacteriostatic diagram of cotton fiber after the cotton fiber and ZnO are loaded.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example 1:
a preparation method of modified nano ZnO antibacterial cellulose fiber and fabric comprises the following steps:
step 1, soaking 2g of cotton fibers in a polycation solution at a soaking temperature of 80 ℃ for 20min at a bath ratio of 1. The preparation method of the polycation solution comprises the following steps: reacting epichlorohydrin with dimethylamine, adding triethylene tetramine, and reacting for 4 hours to obtain a polymer;
step 2, soaking the cellulose fiber or the fabric modified by the polycation into Zn 2+ Adding NaOH solution into zinc ion aqueous solution with the concentration of 40mg/L to control the pH value to be 12, and adding electronegative hydroxyl compound with the dosage of 3g/L to obtain the modified cotton fiber. The preparation method of the electronegative carboxyl group compound comprises the following steps: the molar ratio of 1The carboxyl-terminated compound of (1);
and 3, treating the dipped viscose non-woven fabric by using an ultrasonic transmitter, wherein the ultrasonic frequency is 40kHz, and the ultrasonic time is 5min, so as to obtain the ZnO-loaded antibacterial viscose non-woven fabric.
In this example, the surface of the polycation-modified cellulose fiber was positively charged and had a good affinity for electronegative compounds. The polycation compound and the hydroxyl carboxyl compound have the functions of coating and dispersing the nano material, and the nano ZnO can be loaded on the surface of the fiber by means of ultrasonic energy.
Example 2:
a preparation method of modified nano ZnO antibacterial cellulose fiber and fabric specifically comprises the following steps:
step 1, selecting 60g/m 2 And (3) soaking the viscose spunlace non-woven fabric into a polycation solution, wherein the bath ratio is 1. The preparation method of the polycation solution comprises the following steps: reacting epoxy chloropropane with octadecyl amine, adding amino hyperbranched polymer, heating to 70 ℃, and reacting for 5 hours to obtain a polymer;
step 2, soaking the cellulose fiber or the fabric modified by the polycation into Zn 2+ Adding NaOH solution into zinc ion aqueous solution with the concentration of 40mg/L to control the pH value to be 10, and adding electronegative carboxyl group compound with the dosage of 4g/L to obtain the modified viscose non-woven fabric. The preparation method of the electronegative carboxyl group compound comprises the following steps: polymerizing succinic anhydride and diethanol amine according to a molar ratio of 1;
and 3, treating the impregnated viscose non-woven fabric by using an ultrasonic emitter, wherein the ultrasonic frequency is 40kHz, and the ultrasonic time is 5min, so as to obtain the ZnO loaded antibacterial viscose non-woven fabric.
Example 3:
the nano ZnO-loaded cellulose fibers prepared in examples 1-2 were subjected to electron microscope observation and bacteriostatic experiments.
As shown in fig. 1-2: the structure of the nano ZnO-loaded cellulose fiber prepared in example 1-2 is not substantially different, and as shown in fig. 1, it can be seen that nano ZnO is uniformly loaded on the fiber (nano ZnO content is 2.5 mg/g).
The bacteriostatic experiment steps are as follows: the bacteriostatic effect of the nano-ZnO-loaded cellulose fiber prepared in example 1-2 was determined by referring to the evaluation method of antibacterial performance of GB T20944.3-2008 textile, and the result is shown in FIG. 3.
The antibacterial performance of the nano ZnO-loaded cellulose fibers prepared in examples 1-2 was not substantially different, and as shown in table 1, the inhibition rate = (number of control colonies-number of treated colonies)/number of control colonies × 100%, and it can be seen that the number of treated colonies was less than 20 and the inhibition rate of the nano ZnO-loaded cellulose fibers was more than 99% when the bacteria were grown as they were.
TABLE 1 influence of ZnO Loading and Wash resistance under the action of different additives
As can be seen from Table 1, in the preparation process, under the combined action of the polycation and the electronegative compound, znO can be loaded on the fiber and the fiber has excellent resistance and durability fastness.
In conclusion, the loaded nano ZnO cellulose fiber and fabric prepared by the invention are not easy to harden, have good fluffiness and good nano ZnO dispersibility, and the prepared fiber has good antibacterial property, and the antibacterial rate of the fiber on escherichia coli and staphylococcus aureus can reach more than 99%.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (5)
1. A preparation method of modified nano ZnO antibacterial cellulose fiber and fabric is characterized by comprising the following steps:
step 1, pretreating cellulose fibers; soaking cellulose fiber or fabric into polycation solution at a bath ratio of 1:30, a polycation concentration of 3-10 (o.w.f), a soaking temperature of 40-90 deg.C, and a soaking time of 5-20min;
step 2, soaking the cellulose fiber or the fabric modified by polycation into Zn 2+ Adding alkali liquor into zinc ion aqueous solution with concentration of 40-400mg/L, controlling pH value to 9-12, and selecting electronegative carboxyl or hydroxyl high polymer as stabilizer;
and 3, treating the impregnated cellulose fiber or fabric by using an ultrasonic emitter, wherein the ultrasonic frequency is 20-60kHz, and the ultrasonic time is 5-10min.
2. The method for preparing modified nano ZnO antibacterial cellulose fiber and fabric according to claim 1, wherein in step 1, the cellulose fiber comprises cotton, viscose, modal, lyocell or hemp fiber.
3. The preparation method of the modified nano ZnO antibacterial cellulose fiber and fabric as claimed in claim 1, characterized in that in step 1, the polycation is a cationic compound polymerized from epoxy chloroalkane, secondary amine and tertiary amine.
4. The preparation method of the modified nano ZnO antibacterial cellulose fiber and fabric as claimed in claim 1, wherein in step 2, the aqueous solution of zinc ions is an aqueous solution of zinc nitrate, zinc sulfate or zinc acetate.
5. The method for preparing modified nanometer ZnO antibacterial cellulose fiber and fabric according to claim 1, wherein in step 2, the electronegative high polymer is terminal carboxyl high polymer and terminal carboxyl high polymer with isoelectric point below 6.
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| CN202211437572.7A CN115679681A (en) | 2022-11-17 | 2022-11-17 | Preparation method of modified nano ZnO antibacterial cellulose fiber and fabric |
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| CN202211437572.7A CN115679681A (en) | 2022-11-17 | 2022-11-17 | Preparation method of modified nano ZnO antibacterial cellulose fiber and fabric |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106978722A (en) * | 2017-04-28 | 2017-07-25 | 河南工程学院 | The preparation method of PET non-woven fabrics with photocatalytic degradation function |
| CN107460724A (en) * | 2017-09-17 | 2017-12-12 | 赵兵 | Multifunctional cellulose fiber based on nano zine oxide |
| CN110205800A (en) * | 2019-06-06 | 2019-09-06 | 南通大学 | A kind of preparation method of supported nano zinc oxide alginate fiber and fiber obtained |
| CN113529419A (en) * | 2020-04-17 | 2021-10-22 | 钟春燕 | Bacterial cellulose microfiber-alginic acid fiber composite material loaded with nano zinc oxide |
| US20220331476A1 (en) * | 2020-01-07 | 2022-10-20 | Chunyan Zhong | Nano-zinc oxide-supported bacterial cellulose microfiber-alginate fiber composite |
-
2022
- 2022-11-17 CN CN202211437572.7A patent/CN115679681A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106978722A (en) * | 2017-04-28 | 2017-07-25 | 河南工程学院 | The preparation method of PET non-woven fabrics with photocatalytic degradation function |
| CN107460724A (en) * | 2017-09-17 | 2017-12-12 | 赵兵 | Multifunctional cellulose fiber based on nano zine oxide |
| CN110205800A (en) * | 2019-06-06 | 2019-09-06 | 南通大学 | A kind of preparation method of supported nano zinc oxide alginate fiber and fiber obtained |
| US20220331476A1 (en) * | 2020-01-07 | 2022-10-20 | Chunyan Zhong | Nano-zinc oxide-supported bacterial cellulose microfiber-alginate fiber composite |
| CN113529419A (en) * | 2020-04-17 | 2021-10-22 | 钟春燕 | Bacterial cellulose microfiber-alginic acid fiber composite material loaded with nano zinc oxide |
Non-Patent Citations (1)
| Title |
|---|
| 金丽梅: "《油田废水纳滤处理技术》", vol. 1, 哈尔滨工程大学出版社, pages: 12 - 13 * |
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