CN115874302A - Preparation method of antibacterial degradable fiber, product and application thereof - Google Patents
Preparation method of antibacterial degradable fiber, product and application thereof Download PDFInfo
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- CN115874302A CN115874302A CN202211620671.9A CN202211620671A CN115874302A CN 115874302 A CN115874302 A CN 115874302A CN 202211620671 A CN202211620671 A CN 202211620671A CN 115874302 A CN115874302 A CN 115874302A
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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Abstract
The invention provides a preparation method of antibacterial degradable fiber and a product and application thereof.A zinc salt and urea are dissolved in a mixed solvent of ethylene glycol-deionized water, and are placed in a reaction kettle for reaction, cooling, washing and vacuum drying to obtain zinc hydroxide; putting the mixture into a muffle furnace for calcination to obtain zinc oxide, adding the zinc oxide into silica sol, stirring and mixing the zinc oxide and the silica sol uniformly, adding a silane coupling agent for surface gel reaction, and performing vacuum drying and crushing to obtain porous silica and an inorganic nano powder material subjected to surface modification by the silane coupling agent; and spinning after mixing with the degradable fiber matrix to obtain the antibacterial degradable multifunctional fiber. The invention compounds the antibacterial material and the degradable fiber material, and combines the antibacterial functional component and the degradable fiber base material well, so as to achieve good functionality, spinnability and mechanical strength.
Description
Technical Field
The invention relates to the field of fiber materials, in particular to a preparation method of antibacterial degradable fibers, and a product and application thereof.
Background
The degradable fiber is a fiber material which is spun by degradable polymers and can be completely degraded by organisms in the nature or illumination conditions and the like. The existing commonly used degradable polymers mainly comprise polylactic acid (PLA), polybutylene adipate terephthalate (PBAT), cellulose (CE), chitosan (CS), polycaprolactone (PCL), polyvinyl alcohol (PVA), polyhydroxyalkanoate (PHA), polybutylene succinate (PBS) and the like.
The general problem of degradable fiber materials is that the spinning performance and the mechanical property are slightly inferior compared with other fiber materials. The requirements for introducing other functional ingredients into the degradable fiber are therefore higher than those of other functional fibers. The typical problems are that the mechanical properties of the fiber are seriously deteriorated if other functional ingredients are not well compatible with the degradable fiber base material or are not uniformly dispersed, the use requirement of the fiber material is not met, and the spinning process is easy to break or bond. So that few reports are made on functional degradable fibers at present. The patent CN103668541a and the patent CN111057355a disclose process modification, which solve the above problems, but still can not meet the functional requirements of people for degradable fiber materials. Such as antiviral function, antibacterial function.
The invention provides a preparation method of the antibacterial degradable fiber, and then the antibacterial functional component and the degradable fiber base material are well combined, so that good functionality, spinnability and mechanical strength are achieved at the same time.
Disclosure of Invention
The invention aims to provide a preparation method of an antibacterial degradable fiber, and then antibacterial functional components and a degradable fiber base material are well combined to simultaneously achieve good functionality, spinnability and mechanical strength.
Yet another object of the present invention is to: provides an antibacterial degradable fiber product prepared by the method.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: a preparation method of antibacterial degradable fiber comprises the following steps,
1) Dissolving zinc salt and urea in a mixed solvent of glycol-deionized water, wherein the molar ratio of the zinc salt to the urea is 1 to 3 to 5, and the volume ratio of the glycol to the deionized water is 1 to 3;
2) Placing the mixed solution A in a 100 mL reaction kettle, reacting for 18-24 h at 100-120 ℃, cooling to room temperature, washing 3~5 times by using deionized water and an organic solvent, and drying in a vacuum oven overnight at 100-120 ℃ to obtain zinc hydroxide;
3) Calcining the zinc hydroxide in a muffle furnace at 130 to 200 ℃ for 3 to 5 hours to obtain zinc oxide;
4) Adding the zinc oxide nanoparticles into silica sol, stirring and mixing uniformly, then adding a silane coupling agent for surface gel reaction, drying in vacuum at 120-200 ℃, and crushing to obtain porous silica and an inorganic nano powder material with the surface modified by the silane coupling agent;
5) And (3) mixing the multifunctional nano particles obtained in the step (4) with the degradable fiber matrix, and spinning to obtain the antibacterial degradable multifunctional fiber.
Preferably, in the step 1), the zinc salt is one or a combination of zinc acetate, zinc citrate and zinc formate.
Preferably, in the step 2), the organic solvent is one or a combination of acetone or ethanol.
Preferably, in the step 4), the mass ratio of the inorganic functional nanoparticles to the silica sol is 1:2 to 2:1.
Preferably, in the step 4), the silane coupling agent includes at least one of an alkyl silane coupling agent, a carboxyl silane coupling agent and an aminosilane coupling agent.
Preferably, in the step 5), the degradable fiber matrix comprises at least one of polylactic acid (PLA), polybutylene adipate terephthalate (PBAT), cellulose (CE), chitosan (CS), polycaprolactone (PCL), polyvinyl alcohol (PVA), polyhydroxyalkanoate (PHA), and polybutylene succinate (PBS).
Preferably, in the step 5), the spinning includes solution spinning or melt spinning.
The invention provides an antibacterial degradable fiber prepared by any one of the methods.
The invention provides an application of fiber in preparing an antibacterial degradable fiber material.
Compared with the prior art, the invention has the following beneficial effects:
the invention aims to provide a preparation method of an antibacterial degradable fiber, which is characterized in that an antibacterial material and a degradable fiber material are compounded, and then an antibacterial functional component and a degradable fiber base material are well combined, so that good functionality, spinnability and mechanical strength are achieved at the same time.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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. 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.
The first embodiment is as follows:
an antibacterial degradable fiber is prepared by the following steps:
1) Dissolving zinc salt zinc acetate and urea in a mixed solvent ethylene glycol-deionized water, wherein the molar weight ratio of the zinc acetate to the urea is 1:3, and the volume ratio of the ethylene glycol to the deionized water is 1:1, so as to obtain a mixed solution A;
2) Placing the mixed solution A in a 100 mL reaction kettle, reacting at 100 ℃ for 24 h, cooling to room temperature, washing for 3 times by using deionized water and organic solvent ethanol, and drying in a vacuum oven at 100 ℃ overnight to obtain zinc hydroxide;
3) Calcining the zinc hydroxide in a muffle furnace at 200 ℃ for 3 h to obtain zinc oxide nano particles;
4) Adding the zinc oxide nano particles into silica sol, stirring and mixing uniformly, then adding a silane coupling agent for surface gel reaction, drying in vacuum at 200 ℃, and crushing to obtain porous silica and an inorganic nano powder material with the surface modified by the alkyl silane coupling agent;
5) And (3) mixing the multifunctional nano particles obtained in the step (4) with the degradable fiber matrix, and spinning to obtain the antibacterial degradable multifunctional fiber.
The antibacterial property is excellent by testing, see table 1.
Example two:
an antibacterial degradable fiber is prepared by the following steps similar to the steps of example 1:
1) Dissolving zinc citrate and urea in a mixed solvent of glycol-deionized water, wherein the molar weight ratio of the zinc citrate to the urea is 1:3, and the volume ratio of the glycol to the deionized water is 3:1, so as to obtain a mixed solution A;
2) Placing the mixed solution A in a 100 mL reaction kettle, reacting at 120 ℃ for 18 h, cooling to room temperature, washing for 3 times by deionized water and organic solvent acetone, and drying in a vacuum oven at 100 ℃ overnight to obtain zinc hydroxide;
3) Calcining the zinc hydroxide in a muffle furnace at 130 ℃ for 4 h to obtain zinc oxide nano particles;
4) Adding the zinc oxide nanoparticles into silica sol, stirring and mixing uniformly, then adding a carboxyl silane coupling agent for surface gel reaction, drying in vacuum at 150 ℃, and crushing to obtain porous silica and carboxyl silane coupling agent surface modified inorganic nano powder material;
5) And (5) mixing the multifunctional nanoparticles obtained in the step 4) with the chitosan serving as the degradable fiber matrix, and then carrying out melt spinning to obtain the antibacterial degradable multifunctional fiber.
The antibacterial property is excellent after testing, and is shown in table 1.
Example three:
an antibacterial degradable fiber is prepared by the following steps similar to the steps of example 1:
1) Dissolving zinc formate and urea in a mixed solvent of glycol-deionized water, wherein the molar weight ratio of the zinc formate to the urea is 1:5, and the volume ratio of the glycol to the deionized water is 3:1, so as to obtain a mixed solution A;
2) Placing the mixed solution A in a 100 mL reaction kettle, reacting at 120 ℃ for 18 h, cooling to room temperature, washing for 3 times by using deionized water and organic solvent acetone, and drying in a vacuum oven at 100 ℃ overnight to obtain zinc hydroxide;
3) Calcining the zinc hydroxide in a muffle furnace at 130 ℃ for 4 h to obtain zinc oxide nano particles;
4) Adding the zinc oxide nano particles into silica sol, stirring and mixing uniformly, then adding an aminosilane coupling agent for surface gel reaction, drying in vacuum at 150 ℃, and crushing to obtain porous silica and an inorganic nano powder material with surface modified by the aminosilane coupling agent;
5) And (3) mixing the multifunctional nanoparticles obtained in the step (4) with the degradable fiber matrix polyvinyl alcohol, and then carrying out melt spinning to obtain the antibacterial degradable multifunctional fiber.
The antibacterial property is excellent through testing, and is shown in table 1:
Claims (10)
1. a preparation method of antibacterial degradable fibers is characterized by comprising the following steps,
1) Dissolving zinc salt and urea in a mixed solvent of glycol-deionized water, wherein the molar weight ratio of the zinc salt to the urea is 1:3-5, and the volume ratio of the glycol to the deionized water is 1-3:1, so as to obtain a mixed solution A;
2) Placing the mixed solution A in a 100 mL reaction kettle, reacting at 100-120 ℃ for 18-24 h, cooling to room temperature, washing for 3-5 times by deionized water and an organic solvent, and drying in a vacuum oven at 100-120 ℃ overnight to obtain zinc hydroxide;
3) Calcining the zinc hydroxide in a muffle furnace at 130-200 ℃ for 3-5 h to obtain zinc oxide;
4) Adding the zinc oxide nanoparticles into silica sol, stirring and mixing uniformly, then adding a silane coupling agent for surface gel reaction, drying in vacuum at 120-200 ℃, and crushing to obtain porous silica and an inorganic nano powder material modified by the silane coupling agent;
5) And (3) mixing the multifunctional nano particles obtained in the step (4) with the degradable fiber matrix, and spinning to obtain the antibacterial degradable multifunctional fiber.
2. The method for preparing antibacterial degradable fibers according to claim 1, wherein in step 1), the zinc salt is one or a combination of zinc acetate, zinc citrate and zinc formate.
3. The method for preparing antibacterial degradable fibers according to claim 1, wherein in step 2), the organic solvent is one or a combination of acetone or ethanol.
4. The method for preparing the antibacterial degradable fiber according to claim 1, wherein in the step 4), the mass ratio of the inorganic functional nanoparticles to the silica sol is 1:2-2:1; the silane coupling agent comprises at least one of alkyl silane coupling agent, carboxyl silane coupling agent and amino silane coupling agent.
5. The method for preparing antibacterial degradable fiber according to claim 1, wherein in the step 5), the degradable fiber matrix comprises at least one of polylactic acid (PLA), polybutylene adipate/terephthalate (PBAT), cellulose (CE), chitosan (CS), polycaprolactone (PCL), polyvinyl alcohol (PVA), polyhydroxyalkanoate (PHA), polybutylene succinate (PBS); spinning includes solution spinning or melt spinning.
6. The method for preparing antibacterial degradable fiber according to any one of claims 1 to 5, wherein the method comprises the following steps:
1) Dissolving zinc salt zinc acetate and urea in a mixed solvent ethylene glycol-deionized water, wherein the molar weight ratio of the zinc acetate to the urea is 1:3, and the volume ratio of the ethylene glycol to the deionized water is 1:1, so as to obtain a mixed solution A;
2) Placing the mixed solution A in a 100 mL reaction kettle, reacting at 100 ℃ for 24 h, cooling to room temperature, washing for 3 times by using deionized water and organic solvent ethanol, and drying in a vacuum oven at 100 ℃ overnight to obtain zinc hydroxide;
3) Calcining the zinc hydroxide in a muffle furnace at 200 ℃ for 3 h to obtain zinc oxide nano particles;
4) Adding the zinc oxide nano particles into silica sol, stirring and mixing uniformly, then adding a silane coupling agent for surface gel reaction, drying in vacuum at 200 ℃, and crushing to obtain porous silica and an inorganic nano powder material with the surface modified by the alkyl silane coupling agent;
5) And (5) mixing the multifunctional nano particles obtained in the step 4) with the degradable fiber matrix, and spinning to obtain the antibacterial degradable multifunctional fiber.
7. The method for preparing antibacterial degradable fibers according to any one of claims 1 to 5, wherein the method comprises the following steps:
1) Dissolving zinc citrate and urea in a mixed solvent of glycol-deionized water, wherein the molar weight ratio of the zinc citrate to the urea is 1:3, and the volume ratio of the glycol to the deionized water is 3:1, so as to obtain a mixed solution A;
2) Placing the mixed solution A in a 100 mL reaction kettle, reacting at 120 ℃ for 18 h, cooling to room temperature, washing for 3 times by using deionized water and organic solvent acetone, and drying in a vacuum oven at 100 ℃ overnight to obtain zinc hydroxide;
3) Calcining the zinc hydroxide in a muffle furnace at 130 ℃ for 4 h to obtain zinc oxide nano particles;
4) Adding the zinc oxide nanoparticles into silica sol, stirring and mixing uniformly, then adding a carboxyl silane coupling agent for surface gel reaction, drying in vacuum at 150 ℃, and crushing to obtain porous silica and carboxyl silane coupling agent surface modified inorganic nano powder material;
5) And (3) mixing the multifunctional nanoparticles obtained in the step (4) with the chitosan serving as the degradable fiber matrix, and then carrying out melt spinning to obtain the antibacterial degradable multifunctional fiber.
8. The method for preparing antibacterial degradable fibers according to any one of claims 1 to 5, wherein the method comprises the following steps:
1) Dissolving zinc formate and urea in a mixed solvent of glycol-deionized water, wherein the molar weight ratio of the zinc formate to the urea is 1:5, and the volume ratio of the glycol to the deionized water is 3:1, so as to obtain a mixed solution A;
2) Placing the mixed solution A in a 100 mL reaction kettle, reacting at 120 ℃ for 18 h, cooling to room temperature, washing for 3 times by deionized water and organic solvent acetone, and drying in a vacuum oven at 100 ℃ overnight to obtain zinc hydroxide;
3) Calcining the zinc hydroxide in a muffle furnace at 130 ℃ for 4 h to obtain zinc oxide nano particles;
4) Adding the zinc oxide nano particles into silica sol, stirring and mixing uniformly, then adding an aminosilane coupling agent for surface gel reaction, drying in vacuum at 150 ℃, and crushing to obtain porous silica and an inorganic nano powder material with surface modified by the aminosilane coupling agent;
5) And (3) mixing the multifunctional nanoparticles obtained in the step (4) with the degradable fiber matrix polyvinyl alcohol, and then carrying out melt spinning to obtain the antibacterial degradable multifunctional fiber.
9. An antibacterial degradable fiber characterized by being prepared by the method according to any one of claims 1 to 8.
10. Use of the fiber according to claim 9 for the preparation of an antibacterial degradable fiber material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202211620671.9A CN115874302A (en) | 2022-12-16 | 2022-12-16 | Preparation method of antibacterial degradable fiber, product and application thereof |
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| CN202211620671.9A CN115874302A (en) | 2022-12-16 | 2022-12-16 | Preparation method of antibacterial degradable fiber, product and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116410618A (en) * | 2023-06-12 | 2023-07-11 | 山东工业职业学院 | Synthesis method and application of functionalized modified nano silicon dioxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116410618A (en) * | 2023-06-12 | 2023-07-11 | 山东工业职业学院 | Synthesis method and application of functionalized modified nano silicon dioxide |
| CN116410618B (en) * | 2023-06-12 | 2023-08-18 | 山东工业职业学院 | Synthesis method and application of functionalized modified nano silicon dioxide |
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