CN117844196A - Antibacterial master batch, antibacterial material and preparation method thereof - Google Patents
Antibacterial master batch, antibacterial material and preparation method thereof Download PDFInfo
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 118
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Abstract
The invention discloses an antibacterial master batch, an antibacterial material and a preparation method thereof; the antibacterial master batch comprises an antibacterial agent and a polymer material; the antibacterial agent is selected from A + Y ‑ Any one or more of the following; the antibacterial master batch is prepared by uniformly mixing an antibacterial agent and a polymer material, and then carrying out melt blending, extrusion and granulating in a double-screw extruder. The antibacterial master batch provided by the invention is directly (or after being mixed with matrix resin) subjected to melt spinning to obtain antibacterial fibers or spun-bonded to obtain antibacterial non-woven fabrics, has high antibacterial property and water washing resistance, and is simpler in production process, and the organic antibacterial agent is better in dispersibility and compatibility in the resin; the antibacterial agent of the antibacterial material disclosed by the invention is not easy to fall off, has a good water washing resistance effect, and has a longer-acting antibacterial effect.
Description
Technical Field
The invention belongs to the technical field of fiber fabrics, and particularly relates to an antibacterial masterbatch, an antibacterial material and a preparation method thereof.
Background
The functional antibacterial textile is a novel textile material which can effectively inhibit or kill microorganisms such as bacteria, fungi and the like and has a health care function, not only can effectively prevent the spread and infection of diseases, but also can greatly reduce the cross infection risk of public environment. The fibrous material is the basic unit that makes up the textile, and the realization of many functions of the textile depends on the modification of the fibrous material. The antibacterial function of the textile is closely related to our daily lives. At present, antibacterial materials for textiles mainly comprise inorganic antibacterial agents and organic antibacterial agents.
The inorganic antibacterial agent comprises nano silver, nano copper oxide, nano zinc oxide, nano titanium dioxide and the like, wherein the most commonly used inorganic antibacterial agent is a silver series antibacterial agent. Patent CN105332078B discloses an antibacterial polyester fiber based on silver-loaded zirconium phosphate, which is prepared by in-situ polymerization of silver-loaded zirconium phosphate nano powder and monomer, and is prepared by melt spinning. Patent CN 116240656A discloses an antibacterial master batch prepared based on silver-loaded inorganic antibacterial agent and polymerization doping mixing, and then an antibacterial polyester fiber is obtained through melt spinning, and after the fiber is woven to obtain a fabric, the fabric is immersed in silver-containing solution to obtain the antibacterial fabric. For example, CN104592629A reports a preparation method of a Cu/ZnO-containing composite antibacterial master batch, and the prepared PP slice has good antibacterial property.
However, there are obvious limitations to inorganic antibacterial agents, such as expensive silver-based antibacterial agents, easy discoloration under light, and accumulated toxicity of silver; the inorganic antibacterial agent has poor dispersibility and compatibility in the resin, and can generate agglomeration phenomenon of particles in the granulating or spinning process, thereby influencing the spinnability of the fiber and the strength of the fiber.
For organic antibacterial agents, the antibacterial fibers are prepared by dipping or grafting on the surface of the resin. The patent CN 115852515A sprays a solvent containing 3- (trimethoxy silicon-based) propyl dimethyl octadecyl ammonium chloride on the surface of the polyester filament, and then solidifies the 3- (trimethoxy silicon-based) propyl dimethyl octadecyl ammonium chloride on the surface of the polyester filament by cooling to obtain basic fibers; and drawing and drying the base fiber to obtain the low-sensitization antibacterial polyester fiber. CN 108239881A adopts a co-irradiation grafting method to obtain the antibacterial water-washing-resistant quaternized fiber product. Patent CN111020734B discloses a preparation method of a long-acting antibacterial polyester fiber, firstly, the chemical structure of PHMG is modified by adopting p-carboxylbenzenesulfonamide, and then the modified PHMG reacts with terminal alcohol hydroxyl and ester groups in the polyester fiber, so that the modified PHMG can be used as an antibacterial agent to be added into spinning stock solution, and the prepared polyester fiber has long-term stable and excellent antibacterial performance.
Although the antibacterial agent can be attached to the surface of the fiber through the post-fiber impregnation process treatment, the antibacterial agent is easy to fall off and has poor durability because the antibacterial agent has weak effect on the surface of the fiber. Through the chemical bonding effect, the antibacterial agent can be firmly fixed, the long-acting antibacterial effect is improved, but the production process is complex and the cost is high.
Disclosure of Invention
Based on the defects of the prior art, the invention aims to provide an antibacterial master batch, an antibacterial material and a preparation method thereof; the invention uses the structural formula A + Y - (PF 6 - Or BF 4 - ) The organic antibacterial agent of (2) is prepared by melt spinningThe antibacterial fiber or spun-bonded antibacterial non-woven fabric prepared by the method can obtain antibacterial material with high antibacterial property and washing resistance, has simple process, and also avoids the problem of poor dispersibility and compatibility of inorganic antibacterial agent in resin.
The technical scheme of the invention is as follows:
an antibacterial master batch comprises an antibacterial agent and a polymer material; the antibacterial agent is selected from A + Y - Any one or more of, wherein A + The structure of (1) is that
R 1 、R 2 、R 3 、R 4 Each independently selected from any one of alkyl, phenyl or benzyl with 1-20 carbon atoms; r is alkyl with 1-20 carbon atoms; r is R 5 Is a hydrogen atom or an alkyl group having 1 to 20 carbon atoms;
Y - is of the structure PF 6 - Or BF 4 - 。
Preferably, the alkyl group having 1 to 20 carbon atoms is a linear alkyl group or a branched alkyl group; the alkyl group having 1 to 20 carbon atoms may have 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20 carbon atoms.
Preferably, the antibacterial agent is selected from
(-C 12 H 25 、-C 16 H 33 A linear alkyl group or a branched alkyl group).
More preferably, the antibacterial agent is selected from
Preferably, the polymeric material is selected from one or more of polyethylene, polypropylene, polyvinyl chloride, polyamide, polyester and polyurethane.
More preferably, the polyamide comprises one or more of polyamide-6 and polyamide-66.
More preferably, the polyester comprises one or more of polyethylene terephthalate, polybutylene terephthalate, and polycyclohexane dimethyl terephthalate.
Preferably, the mass content of the antibacterial agent in the antibacterial master batch is 0.1-20wt%.
The preparation method of the antibacterial master batch comprises the following steps:
and after uniformly mixing the antibacterial agent and the polymer material, carrying out melt blending, extrusion and granulating in a double-screw extruder to prepare the antibacterial master batch.
Preferably, the temperature of the melt blending is 180-280 ℃.
The antibacterial material comprises the following components in parts by weight:
0-98 parts of matrix resin;
2-100 parts of the antibacterial master batch;
the mass content of the antibacterial agent in the antibacterial material is 0.1-5 wt%.
Preferably, the matrix resin is selected from one or more of polyethylene, polypropylene, polyvinyl chloride, polyamide, polyester and polyurethane.
More preferably, the polyamide comprises one or more of polyamide-6 and polyamide-66.
More preferably, the polyester comprises one or more of polyethylene terephthalate, polybutylene terephthalate, and polycyclohexane dimethyl terephthalate.
Preferably, the antibacterial material is antibacterial fiber or antibacterial non-woven fabric.
The preparation method of the antibacterial material comprises the following steps:
mixing antibacterial master batches with matrix resin, and performing melt spinning to obtain antibacterial fibers;
mixing the antibacterial master batch with matrix resin, and performing spunbonding to obtain the antibacterial non-woven fabric.
Preferably, the temperature of the melt spinning is 200-280 ℃, and the winding rate of the melt spinning is 900-1200m/min;
preferably, the spunbond temperature is 200-280 ℃.
The invention has the advantages and beneficial effects that:
(1) The structural formula of the invention is A + Y - (PF 6 - Or BF 4 - ) The organic antibacterial agent and the resin are melt blended, extruded and granulated to obtain antibacterial master batches;
(2) The antibacterial master batch is directly (or after being mixed with matrix resin) subjected to melt spinning to obtain antibacterial fibers, or is subjected to melt blowing or spun bonding to obtain antibacterial non-woven fabrics, so that the antibacterial master batch has high antibacterial property and water washing resistance, the production process is simpler, and the dispersibility and compatibility of the organic antibacterial agent in the resin are better;
(3) The antibacterial agent of the antibacterial material disclosed by the invention is not easy to fall off, has a good water washing resistance effect, and has a longer-acting antibacterial effect.
Detailed Description
Specific embodiments of the present invention will be further described below with reference to examples, but the practice and protection of the present invention are not limited thereto. It should be noted that the following processes, if not specifically described in detail, can be realized or understood by those skilled in the art with reference to the prior art. The reagents or apparatus used were not manufacturer-specific and were considered conventional products commercially available.
The following antibacterial agents refer to alkyl chains (e.g. -C 12 H 25 、C 16 H 33 ) Are all straight chain alkyl groups.
The following examples and comparative examples were prepared by the following methods for DAPF6, DTAPF6, CPPF6, BMIPF6, BBRBF4, CTABF4, and CTAPF 6:
(1) The preparation method of the DAPF6 comprises the following steps:
molecular DAC was used at 25℃at room temperatureDissolving with water and filtering to obtain saturated solution of DAC, adding saturated aqueous solution of potassium hexafluorophosphate with mass ratio (mass of saturated aqueous solution of potassium hexafluorophosphate/mass of saturated solution of DAC) of 0.5, stirring, filtering to obtain precipitate, and oven drying to obtain DAPF 6->
(2) The preparation method of the DTAPF6 comprises the following steps:
the molecule DTAB was subjected to room temperature at 25 DEG CDissolving with water and filtering to obtain saturated solution of DTAB, adding saturated aqueous solution of potassium hexafluorophosphate with mass ratio (mass of saturated aqueous solution of potassium hexafluorophosphate/mass of saturated solution of DTAB) of 0.4, stirring, filtering, precipitating, and oven drying to obtain DTAPF 6->
(3) The preparation method of CPPF6 comprises the following steps:
molecular CPC at 25deg.C at room temperatureDissolving with water and filtering to obtain saturated solution of CPC, adding saturated aqueous solution of potassium hexafluorophosphate with mass ratio (mass of saturated aqueous solution of potassium hexafluorophosphate/mass of saturated solution of CPC) of 0.4, stirring, filtering, precipitating, and oven drying to obtain CPPF 6->
(4) The preparation method of BMIPF6 comprises the following steps:
molecular BMIC was incubated at 25℃at room temperatureDissolving with water and filtering to obtain saturated solution of BMIC, adding saturated aqueous solution of potassium hexafluorophosphate with mass ratio (mass of saturated aqueous solution of potassium hexafluorophosphate/mass of saturated solution of BMIC) of 0.4, stirring, filtering, precipitating, and oven drying to obtain BMIPF6
(5) The preparation method of BBRBF4 comprises the following steps:
the molecular BBR is subjected to room temperature at 25 DEG CDissolving with methanol and filtering to obtain saturated solution of BBR, adding saturated aqueous solution of sodium tetraborate phosphate with mass ratio (mass of saturated aqueous solution of sodium tetrafluoroborate/mass of saturated solution of BBR) of 0.4, stirring, filtering, precipitating, and oven drying to obtain BBRBF 4->
(6) The preparation method of CTABF4 comprises the following steps:
molecular CTAC at 25℃at room temperatureDissolving with water and filtering to obtain saturated solution of CTAC, adding saturated solution of sodium tetraborate phosphate with mass ratio (mass of saturated aqueous solution of sodium tetrafluoroborate/mass of saturated solution of CTAC) of 0.4, stirring, filtering, precipitating, and oven drying to obtain CTABF 4->
(7) The preparation method of CTAPF6 comprises the following steps:
molecular CTAC at 25℃at room temperatureDissolving with water and filtering to obtain saturated solution of CTAC, adding saturated aqueous solution of potassium hexafluorophosphate with mass ratio (mass of saturated aqueous solution of potassium hexafluorophosphate/mass of saturated solution of CTAC) of 0.4, stirring, filtering, precipitating, and oven drying to obtain CTAPF 6->
Example 1:
taking 2kg of antibacterial agent DAPF6Mixing with 38kg of polyethylene terephthalate, and carrying out melt blending, extrusion and granulating in a double-screw extruder to obtain antibacterial master batches; taking 20kg of antibacterial master batch, and preparing fibers by melt spinning; the temperature of melt blending was 260 ℃, the temperature of melt spinning was 280 ℃, and the winding rate in melt spinning was 1150m/min.
Example 2:
1kg of antimicrobial DTAPF6 is takenMixing with 19kg of polyamide-6, and carrying out melt blending, extrusion and granulating in a double-screw extruder to obtain antibacterial master batches; taking 4kg of antibacterial master batch, mixing with 16kg of common polyamide-6 resin, and preparing fibers by melt spinning; the temperature of melt blending was 250 ℃, the temperature of melt spinning was 250 ℃, and the winding rate in melt spinning was 1150m/min.
Example 3:
taking 0.1kg of antibacterial agent CPPF6Mixing with 1.9kg of polyurethane, and carrying out melt blending, extrusion and granulating in a double-screw extruder to obtain antibacterial master batches; taking 0.4kg of antibacterial master batch, mixing with 19.6kg of polyurethane resin, and preparing fibers by melt spinning; the temperature of melt blending isThe temperature of the melt spinning was 220℃and the winding rate in the melt spinning was 1150m/min.
Example 4:
1kg of the antibacterial agent BMIPF6 was takenMixing with 19kg of polypropylene, and carrying out melt blending, extrusion and granulating in a double-screw extruder to obtain antibacterial master batches; taking 8kg of antibacterial master batch, mixing with 12kg of polypropylene resin, and preparing an antibacterial non-woven fabric by spunbonding; the melt blending temperature was 230℃and the spunbond temperature was 230 ℃.
Example 5:
taking 1kg of antibacterial BBRBF4Mixing with 19kg of polypropylene, and carrying out melt blending, extrusion and granulating in a double-screw extruder to obtain antibacterial master batches; taking 8kg of antibacterial master batch, mixing with 12kg of polypropylene resin, and preparing an antibacterial non-woven fabric by spunbonding; the melt blending temperature was 230℃and the spunbond temperature was 230 ℃.
Example 6:
1kg of antibacterial agent CTABF4 is takenMixing with 19kg of polypropylene, and carrying out melt blending, extrusion and granulating in a double-screw extruder to obtain antibacterial master batches; taking 8kg of antibacterial master batch, mixing with 12kg of polypropylene resin, and preparing an antibacterial non-woven fabric by spunbonding; the melt blending temperature was 230℃and the spunbond temperature was 230 ℃.
Example 7:
1kg of antibacterial agent CTAPF6 is takenMixing with 19kg of polypropylene, and carrying out melt blending, extrusion and granulating in a double-screw extruder to obtain antibacterial master batches; taking 8kg of antibacterial master batch, mixing with 12kg of polypropylene resin, and preparing an antibacterial non-woven fabric by spunbonding; the melt blending temperature was 230℃and the spunbond temperature was 230 ℃.
Comparative example 1:
taking 2kg of antibacterial DACMixing with 38kg of polyethylene terephthalate, and carrying out melt blending, extrusion and granulating in a double-screw extruder to obtain antibacterial master batches; taking 20kg of antibacterial master batch, and preparing fibers by melt spinning; the temperature of melt blending was 260 ℃, the temperature of melt spinning was 280 ℃, and the winding rate in melt spinning was 1150m/min.
Comparative example 2:
1kg of antimicrobial DTAB is takenMixing with 19kg of polyamide-6, and carrying out melt blending, extrusion and granulating in a double-screw extruder to obtain antibacterial master batches; taking 4kg of antibacterial master batch, mixing with 16kg of common polyamide-6 resin, and preparing fibers by melt spinning; the temperature of melt blending was 250 ℃, the temperature of melt spinning was 250 ℃, and the winding rate in melt spinning was 1150m/min.
Comparative example 3:
taking 0.1kg of antibacterial agent CPCMixing with 1.9kg of polyurethane, and carrying out melt blending, extrusion and granulating in a double-screw extruder to obtain antibacterial master batches; taking 0.4kg of antibacterial master batch, mixing with 19.6kg of polyurethane resin, and preparing fibers by melt spinning; the temperature of melt blending was 220 ℃, the temperature of melt spinning was 220 ℃, and the winding rate in melt spinning was 1150m/min.
Comparative example 4:
1kg of the antibacterial agent BMIC was takenMixing with 19kg of polypropylene, and carrying out melt blending, extrusion and granulating in a double-screw extruder to obtain antibacterial master batches; taking 8kg of antibacterial master batch, mixing with 12kg of polypropylene resin, and preparing an antibacterial non-woven fabric by spunbonding; melt blendingThe temperature of (2) was 230℃and the spunbond temperature was 230 ℃.
Comparative example 5:
taking 1kg of antibacterial BBRMixing with 19kg of polypropylene, and carrying out melt blending, extrusion and granulating in a double-screw extruder to obtain antibacterial master batches; taking 8kg of antibacterial master batch, mixing with 12kg of polypropylene resin, and preparing an antibacterial non-woven fabric by spunbonding; the melt blending temperature was 230℃and the spunbond temperature was 230 ℃.
Comparative example 6:
antibacterial agent BBRBF4Dissolving in THF/water mixed solvent to prepare 2% BBRBF4 antibacterial agent finishing liquid, soaking non-woven fabric prepared by a spunbonding process (the spunbonding temperature is 230 ℃) with polypropylene in the BBRBF4 antibacterial agent finishing liquid, taking out, and drying to obtain the antibacterial non-woven fabric.
Comparative example 7:
1kg of antibacterial agent CTAC was takenMixing with 19kg of polypropylene, and carrying out melt blending, extrusion and granulating in a double-screw extruder to obtain antibacterial master batches; taking 8kg of antibacterial master batch, mixing with 12kg of polypropylene resin, and preparing an antibacterial non-woven fabric by spunbonding; the melt blending temperature was 230℃and the spunbond temperature was 230 ℃.
Testing and result analysis:
testing according to GB/T20944.3-2008 (part 2 in evaluation of antibacterial property of textile: vibration method), wherein the test strain is staphylococcus aureus; the test results are shown in Table 1.
TABLE 1
From the experimental results of the antibacterial properties of the fibers and the nonwoven fabrics, it can be seen that the antibacterial rates of the fibers/nonwoven fabrics of comparative examples 1 to 5 and comparative example 7 were 12%, 0, 5%, 21%, 18% and 35%, respectively, whereas the antibacterial rates of the fibers/fabrics prepared in examples 1 to 7 using the antibacterial agent of the present invention were >99%, 97%, 99% and 99%, respectively, which were higher than those of comparative examples, and have remarkable antibacterial effects. While the antibacterial agent of the present invention was used in comparative example 6 after 100 washes, the antibacterial rate of the nonwoven fabrics prepared by different processes was reduced from >99% to 36%, and the antibacterial rate was maintained at least to 95% after 100 washes in examples 1 to 7, indicating that the antibacterial performance of the fiber/nonwoven fabrics prepared by the technique of the present invention had a good water-washing resistance.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (10)
1. An antibacterial master batch is characterized by comprising an antibacterial agent and a polymer material; the antibacterial agent is selected from A + Y - Any one or more of, wherein A + The structure of (1) is that
R 1 、R 2 、R 3 、R 4 Each independently selected from any one of alkyl, phenyl or benzyl with 1-20 carbon atoms; r is alkyl with 1-20 carbon atoms; r is R 5 Is hydrogen or C1-20An alkyl group;
Y - is of the structure PF 6 - Or BF 4 - 。
2. The antimicrobial master batch of claim 1, wherein the antimicrobial agent is selected from the group consisting of
Any one or more of the following.
3. The antimicrobial masterbatch of claim 1 wherein the polymeric material is selected from one or more of polyethylene, polypropylene, polyvinyl chloride, polyamide, polyester, and polyurethane.
4. The antimicrobial masterbatch of claim 3 wherein the polyamide comprises one or more of polyamide-6 and polyamide-66; the polyester comprises one or more of polyethylene terephthalate, polybutylene terephthalate, and polybutylene terephthalate.
5. The antibacterial master batch according to claim 1, wherein the mass content of the antibacterial agent in the antibacterial master batch is 0.1-20wt%.
6. The method for producing an antibacterial master batch according to any one of claims 1 to 5, comprising the steps of:
and after uniformly mixing the antibacterial agent and the polymer material, carrying out melt blending, extrusion and granulating in a double-screw extruder to prepare the antibacterial master batch.
7. The antibacterial material is characterized by comprising the following components in parts by weight:
0-98 parts of matrix resin;
2-100 parts of the antibacterial masterbatch according to any one of claims 1 to 5;
the mass content of the antibacterial agent in the antibacterial material is 0.1-5 wt%.
8. The antimicrobial material of claim 7, wherein the matrix resin is selected from one or more of polyethylene, polypropylene, polyvinyl chloride, polyamide, polyester, and polyurethane.
9. The antimicrobial material of claim 7, wherein the antimicrobial material is an antimicrobial fiber or an antimicrobial nonwoven.
10. A method for producing an antibacterial material according to any one of claims 7 to 9, comprising the steps of:
mixing antibacterial master batches with matrix resin, and performing melt spinning to obtain antibacterial fibers;
mixing the antibacterial master batch with matrix resin, and performing spunbonding to obtain the antibacterial non-woven fabric.
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| CN202311742646.2A CN117844196A (en) | 2023-12-18 | 2023-12-18 | Antibacterial master batch, antibacterial material and preparation method thereof |
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| CN202311742646.2A CN117844196A (en) | 2023-12-18 | 2023-12-18 | Antibacterial master batch, antibacterial material and preparation method thereof |
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