CN101987885A - Antibacterial, waterproof and moisture permeable type composite functional material and preparation method and application thereof - Google Patents
Antibacterial, waterproof and moisture permeable type composite functional material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an antibacterial, waterproof and moisture permeable type composite functional material, which comprises the following components in part by weight: 92 to 98 parts of waterproof and moisture permeable polyurethane and 2 to 8 parts of nano antibacterial particles. The preparation method for the composite functional material comprises the following steps of: 1) chemically modifying the nano antibacterial particles; 2) preparing a performed polymer of waterproof and moisture permeable type functional polyurethane; and 3) performing chemical grafting reaction on the nano antibacterial particles which are chemically modified and the waterproof and moisture permeable type functional polyurethane to finally obtain the antibacterial, waterproof and moisture permeable polyurethane/nano antibacterial particle composite functional material of the invention. The functional material interacts with fabrics to be prepared into antibacterial, waterproof and moisture permeable type medical protection clothing products by coating technology, and tests prove that medical protection clothing has higher antibacterial, waterproof and moisture permeable performance.
Description
Technical field
The present invention relates to a kind of antibiotic Waterproof Breathable composite functional material, be specifically related to a kind of waterproof moisture-penetrating urethane (PU)/nano-antibacterial particle (NAP) composite functional material and preparation method thereof, the invention still further relates to the application of this waterproof moisture-penetrating urethane (PU)/nano-antibacterial particle (NAP) composite functional material aspect the preparation medical protective garment.
Background technology
At present, the water proof and moisture permeable material that is applied to fabric laminated or coating mainly contains two class main flow materials, and a class is the polytetrafluoroethylene (PTFE) film, and another kind of is block polyurethane (PU) emulsion and film.
Wherein, PTFE mainly carries out the lamination arrangement with laminated mode and fabric.The PTFE film have two generation product, first-generation product is a microporous membrane, the diameter of micropore is much smaller than the diameter (200 μ m) of water droplet or droplet, but much larger than the diameter (0.4 * 10 of steam
-4μ m), thus realize Waterproof Breathable.Because the inertia of PTFE itself, can not carry out good bondingly with fabric, for this reason, developed s-generation PTFE film.During use generally with PTFE film and the hydrophilic film laminated film that becomes laminated together, the moisture permeation mechanism of this moment is, " the chemical ladder stone " of hydrophilic radical effect in the hydrophilic film molecule, promptly by absorption-diffusion-desorption mode, water vapour molecule along ladder from high humidity one side move to low humidity one side, carry out wet.Though the waterproofing and moisture-penetration performances of PTFE lining is outstanding, because such film is difficult to be degraded by nature, the large-scale application makes PTFE become the killer of environment gradually.Therefore, in today that environmentalism is propagated its belief on a large scale, PTFE is faced with the crisis of environmental protection.And the PTFE price is expensive, and after the PTFE arrangement, the flexibility of fabric and drape are also unsatisfactory.
Therefore PU emulsion or film are to prepare waterproof moisture permeating fabric with coating or laminated technology, contain a large amount of polar groups in the PU macromole, and Intermolecular Forces is very strong, have good film-forming properties, and can carry out good bonding with fabric.The PU coating is a nonporous film, and the continuity of film makes it have excellent water-repellancy, and moisture permeation mechanism then acts on simultaneously with " chemical ladder stone " dual mode of " function micropore " and hydrophilic radical.Polar group or hydrophilic radical among the one side PU, as-OH ,-NHCOO-,-SO
3H ,-" chemical ladder stone " effect of COOH etc., make water vapour molecule along ladder from high humidity one side move to low humidity one side; PU is made up of soft chain segment (but anti-phase) and hard segment (stationary phase) on the other hand, wherein stationary phase has high glass transition (Tg) and crystalline melt temperature (Tm), but and anti-phase at 15 ℃--tangible second-order transition temperature (Tg) and crystalline melt temperature (Tm) are arranged in 60 ℃ of temperature ranges.If Tg or Tm are set at the comfort temperature of human body requirements, when envrionment temperature was lower than Tg or Tm, the motion of polymer molecule segment was frozen, and polymkeric substance is in crystal form or vitreous state, and the densification of molecular chain is arranged and made vapor transfer rate less; And when envrionment temperature was higher than Tg or Tm, the macromolecular chain segment of polymkeric substance thawed and is in rubbery state, and high molecular interchain gap (free volume) obviously increases, thereby had high vapor transfer rate.This water vapour permeability of block function PU material is that snugness of fit can be regulated voluntarily by the variation of human body or ambient temperature, has intelligentized effect.
Therefore, PU coating or lamination have can with good bonding of fabric, the continuity of non-porous film makes it have excellent water-repellancy, but the block chemical structure that stationary phase and anti-phase constitute makes it pass through " function micropore " and " chemical ladder stone " dual mode and realizes water vapour permeability, and this water vapour permeability has intelligentized effect and price is lower.In addition, the PU emulsion has reduced the use of organic solvent, environmental protection.The more important thing is that PU is than PTFE low price.
For the multifunction research of waterproof moisture permeating fabric, that is: make waterproof moisture permeating fabric have the development of specific functions such as antibiotic, warming, fire-retardant, antistatic, anti-ultraviolet simultaneously at present, also be in the starting stage both at home and abroad now.Obtaining Waterproof Breathable function and other function compound approach great majority adopts function nano particle and water proof and moisture permeable material to carry out the form of physical blending, this method occurs nanoparticle easily and disperses inhomogeneous, reunion, inorganic nano-particle and polymer phase capacitive are bad, and the phenomenons such as mechanical property that influence water proof and moisture permeable material, so its application also just is subjected to certain restriction.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of antibiotic waterproof moisture-penetrating urethane (PU)/nano-antibacterial particle (NAP) composite functional material and its production and application, utilize inorganic/organic hybrid theory, after function nano antimicrobial particle (NAP) carried out finishing, with its with the chemical bond grafting to Waterproof Breathable PU material, thereby good improve the function nano dispersion of particles and and polymkeric substance between consistency, obtain the persistent antibiotic Waterproof Breathable complex function fabric of function, adopt coating technology at last again, the complex function textile that is obtained is become antibiotic Waterproof Breathable medical protective garment product.
For achieving the above object, the present invention realizes by the following technical solutions:
A kind of antibiotic Waterproof Breathable composite functional material comprises following components in part by weight:
Waterproof moisture-penetrating urethane (PU) 92-98 part;
Nano-antibacterial particle (NAP) 2-8 part.
Described waterproof moisture-penetrating urethane is prepared from by polyvalent alcohol, binary or multicomponent isocyanate and chainextender.
Described polyvalent alcohol is polyether-type or polyester type.
Described binary or multicomponent isocyanate are aromatic series, aliphatics or alicyclic.
Described chainextender is small molecules glycol or two amines.
Described nano-antibacterial particle is a nanometer Ag
+, its particle diameter is 10-80nm.
The preparation method of above-mentioned antibiotic Waterproof Breathable composite functional material may further comprise the steps:
1) the nano-antibacterial particle is carried out chemically modified, make its stable being dispersed in the water, and by the activation of the coupling agent of bifunctional, form the A component, its chemical equation is as follows:
The A component
Wherein, NAP represents the nano-antibacterial particle;
2) to the synthetic Molecular Structure Design of carrying out of urethane, the soft segment molecule amount that preparation is suitable and the block polyurethane performed polymer of hard segment content, and introduce hydrophilic ionic group so that it can carry out the emulsification chain extension in water in hard section, make polyurethane material with Waterproof Breathable function, be the B component, its chemical equation is as follows:
The B component
Wherein, DBTDL is the catalyzer dibutyl tin laurate, and DMPA is an organic solvent 2, and 2-dimethylol propionic acid, BDO are chainextender 1, the 4-butyleneglycol;
3) the A component is dispersed in the aqueous solution of triethylamine, forms the C component;
4) the B component is joined in the C component, carry out emulsification, chain extension and graft reaction, with ketoxime unreacted isocyanic ester is carried out end-blocking then, promptly make the PU/NAP composite functional material, its chemical equation is as follows:
Among the above-mentioned preparation method, wherein, the coupling agent of described bifunctional is N-β-(aminoethyl)-γ-An Bingjisanjiayangjiguiwan, the domestic corresponding trade mark: the KH-792 of the Chinese Academy of Sciences, the external corresponding trade mark: U.S. union carbide corporation A-1120; The Z-6020 of Dow corning company; The KBM-603 of Japan XINYUE.
Among the above-mentioned preparation method, wherein, described soft segment of polyurethane is 1 with the mass ratio of hard section: 2.5-1: 4, and wherein hard section is micromolecular dibasic alcohol, perhaps the aromatic diisocyanate of diamine connection; Soft section is polyether Glycols or polyester diol.
Among the above-mentioned preparation method, wherein, described ketoxime is a Diacetylmonoxime.
The application of described antibiotic Waterproof Breathable composite functional material aspect fabric, promptly select ketoxime organic micromolecule for use with active-H group, as Diacetylmonoxime, urethane/antimicrobial nano particle mixture performed polymer is carried out end capping, and when fabric carried out coating, attemperation is with end capped isocyanic ester deblocking, generate the carboxylamine ester structure with the hydroxyl-OH reaction on the fabric, generate chemical bond and reach firm adhesive effect between urethane/antimicrobial nano particle mixture and fabric, its chemical equation is as follows:
The application of described antibiotic Waterproof Breathable composite functional material in the preparation medical protective garment.
In general, described PU coating and laminated water vapour permeability working mechanism have following several (referring to Fig. 2):
(a) micropore moisture permeation mechanism
(b) chemical ladder stone moisture permeation mechanism
(c) the saturating mechanism of the intelligent functions of PU material
Thereby Waterproof Breathable function PU material is widely used in coated fabric.The continuity of PU film makes fabric have excellent water-repellancy; The water vapour permeability of PU film is acted on simultaneously by " function micropore " and " chemical ladder stone " dual mode.Prepare by soft section and hard section block PU that forms by molecular designing, soft section chemical structure has good hydrophilicity, perviousness and certain chain length, make that soft section Tm or Tg value are the comfort temperature value of human body requirements, thereby when outside temperature is lower than Tm or Tg value, has low vapor transfer rate, insulation that can be suitable; When outside temperature was higher than Tm or Tg value, fabric presented high water vapour permeability, can quicken heat radiation and perspire.The characteristic that this vapor transfer rate can be regulated along with the variation of outside temperature is that the intellectuality of Waterproof Breathable function PU embodies.
In addition, the PU material is using and is depositing in the process, very easily grows under suitable temperature and humidity condition and breeds bacterium, serious threat people's health.Therefore, the Waterproof Breathable function PU material of preparation anti-microbial property is instant, is to satisfy the comfortable and easy to wear and healthy prerequisite of people.Among the present invention, nano antibacterial agent NAP is grafted on the PU material by chemical reaction, overcome antiseptic-germicide and PU inhomogeneous with the dispersion that addition manner was occurred of physical blending, the phenomenon of consistency difference.Can obtain durable antibiotic, Waterproof Breathable PU composite functional material.
The present invention combines intellectuality and the multifunction of function PU, make the PU/NAP composite functional material, and be applied in the product development of antibiotic Waterproof Breathable functional type medical protective garment, realized that medical protective garment must have barrier propterty and wet thoroughly comfort property antibiotic, waterproof concurrently, avoided the medical protective garment in SARS period, medical personnel soon will be soaked with sweat after dressing, some medical workers are owing to wear this protective clothing for a long time, even uncomfortable in chest, collapse phenomenon occurs, thereby influence the phenomenon of curative activity.
PU/NAP composite functional material of the present invention is widely used in the production of medical textile, to satisfy the comfortable and easy to wear and healthy demand of people.Simultaneously, the Application Areas of PU/NAP also can expand footwear industries, civil or military project uniform and the clothes under extreme weather conditions, anti-oilcloth, tent, parcel etc. to, along with the human knowledge and the further enhancing of ability that conquers nature, thereby satisfy the operation of people under particular surroundings.
Description of drawings
Fig. 1 is the conformational map of PU/NAP hydridization type composite functional material of the present invention.
Embodiment
Embodiment 1
The finishing of nano-antibacterial particle
Get the nano-antibacterial Ag of 2g
+Particle (particle diameter 30nm) is dissolved in it in second distillation aqueous solution of 100ml, adds the coupling agent KH-792 of 0.5g under the room temperature, stir 4h, sedimentation and filtration, and the nano-antibacterial particle A component that has promptly obtained being activated, standby.
Embodiment 2
Synthesizing of polyaminoester emulsion
Metering polyvalent alcohol PPG after the vacuum-drying is joined in the there-necked flask that reflux condensing tube, temperature controller and agitator are housed N
2Protection drips the vulcabond that measures down, and (TD I: MD I-100HL mass ratio=9: 1) mixture carries out just poly-reaction, and temperature of reaction maintains 80 ℃.Be reacted to a certain degree to the faint yellow and slightly general green glow of emulsion appearance, introduce self-emulsifier/hydrophilic radical DMPA (in advance with an amount of NMP dissolving) and chainextender BD, under 75 ℃ of conditions, carry out chain extending reaction, add small amount of acetone in the reaction process and reduce viscosity.After chain extending reaction is finished, be cooled to 45 ℃, reaction product is poured in the beaker, be placed in the mulser and stir, the deionized water that is dissolved with neutralizing agent TEA is slowly added, emulsive neutralizes simultaneously.After fully emulsified, acetone is removed in underpressure distillation, makes polyaminoester emulsion, i.e. the B1 component.
Embodiment 3
Synthesizing of polyaminoester emulsion
Metering polyvalent alcohol PEG after the vacuum-drying is joined in the there-necked flask that reflux condensing tube, temperature controller and agitator are housed N
2Protection drips the vulcabond that measures down, and (TDI: MD I-100HL mass ratio=9: 1) mixture carries out just poly-reaction, and temperature of reaction maintains 80 ℃.Be reacted to a certain degree to the faint yellow and slightly general green glow of emulsion appearance, introduce self-emulsifier/hydrophilic radical DMPA (in advance with an amount of NMP dissolving) and chainextender BD, under 75 ℃ of conditions, carry out chain extending reaction, add small amount of acetone in the reaction process and reduce viscosity.After chain extending reaction is finished, be cooled to 45 ℃, reaction product is poured in the beaker, be placed in the mulser and stir, the deionized water that is dissolved with neutralizing agent TEA is slowly added, emulsive neutralizes simultaneously.After fully emulsified, acetone is removed in underpressure distillation, makes polyaminoester emulsion, i.e. the B2 component.
Embodiment 4
The preparation of PU/NAP composite functional material
A component among the embodiment 1 is distributed in the aqueous solution of triethylamine, form the C component, then the B1 component among the embodiment 2 is added in the C component, wherein the weight of A, B component is respectively 2 parts and 98 parts, carry out emulsification, chain extension and graft reaction, with ketoxime unreacted isocyanic ester is carried out end-blocking at last, promptly make polyurethane/nano antimicrobial particle composite functional material.
Embodiment 5
The preparation of PU/NAP composite functional material
A component among the embodiment 1 is distributed in the aqueous solution of triethylamine, form the C component, then the B2 component among the embodiment 3 is added in the C component, wherein the weight of A, B component is respectively 8 parts and 92 parts, carry out emulsification, chain extension and graft reaction, with ketoxime unreacted isocyanic ester is carried out end-blocking at last, promptly make polyurethane/nano antimicrobial particle composite functional material.
Embodiment 6
The application of PU/NAP composite functional material
PU/NAP composite functional material and fourth oximinoketone that weight fraction is respectively 95 parts, 6 parts react 2h under 60 ℃, add textile cloth when then temperature being elevated to 150 ℃, be prepared into antibiotic Waterproof Breathable medical protective garment product by coating or lamination.
Antibiotic Waterproof Breathable functional type medical protective garment to above-mentioned preparation carries out anti-microbial property, water resistance, water vapour permeability test, and its examination criteria and performance index are as shown in table 1, and the result is as shown in table 2.
Table 1
Annotate: the selected bacterium of antibacterial experiment of the present invention is: gram-positive microorganism and Gram-negative bacteria.Wherein gram-positive microorganism comprises: Bacillus cereus, Corynebacterium pseudodi phtheriae, drug resistance of vancomycin faecalis staphylococcus aureus, staphylococcus epidermidis; Gram-negative bacteria comprises: Acinetobacter baumannii, intestinal bacteria, pneumonia Ke Bailei bacillus (ATCC4352), pseudomonas aeruginosa, Salmonella choleraesuls.
Table 2
As can be seen from Table 2, antibiotic Waterproof Breathable PU/NAP composite functional material of the present invention has good antibiotic, waterproof and water vapour permeability, can be widely used in the production of medical textile.
Claims (12)
1. an antibiotic Waterproof Breathable composite functional material is characterized in that, comprises following components in part by weight:
Waterproof moisture-penetrating urethane 92-98 part;
Nano-antibacterial particle 2-8 part.
2. antibiotic Waterproof Breathable composite functional material according to claim 1 is characterized in that described waterproof moisture-penetrating urethane is prepared from by polyvalent alcohol, binary or multicomponent isocyanate and chainextender.
3. antibiotic Waterproof Breathable composite functional material according to claim 2 is characterized in that described polyvalent alcohol is polyether-type or polyester type.
4. antibiotic Waterproof Breathable composite functional material according to claim 2 is characterized in that, described binary or multicomponent isocyanate are aromatic series, aliphatics or alicyclic.
5. antibiotic Waterproof Breathable composite functional material according to claim 2 is characterized in that, described chainextender is small molecules glycol or two amines.
6. antibiotic Waterproof Breathable composite functional material according to claim 1 is characterized in that described nano-antibacterial particle is a nanometer Ag
+, its particle diameter is 10-80nm.
7. method for preparing antibiotic Waterproof Breathable composite functional material as claimed in claim 1 may further comprise the steps:
1) the nano-antibacterial particle is carried out chemically modified, make its stable being dispersed in the water, and by the activation of the coupling agent of bifunctional, form the A component, its chemical equation is as follows:
Wherein, the NAP in the following formula is the nano-antibacterial particle;
2) to the synthetic Molecular Structure Design of carrying out of urethane, the soft segment molecule amount that preparation is suitable and the block polyurethane performed polymer of hard segment content, and introduce hydrophilic ionic group so that it can carry out the emulsification chain extension in water in hard section, make polyurethane material with Waterproof Breathable function, be the B component, its chemical equation is as follows:
Wherein, DBTDL is the catalyzer dibutyl tin laurate, and DMPA is an organic solvent 2, and 2-dimethylol propionic acid, BDO are chainextender 1, the 4-butyleneglycol;
3) the A component is dispersed in the aqueous solution of triethylamine, forms the C component;
4) the B component is joined in the C component, carry out emulsification, chain extension and graft reaction, with ketoxime unreacted isocyanic ester is carried out end-blocking then, promptly make polyurethane/nano antimicrobial particle composite functional material, its chemical equation is as follows:
8. preparation method according to claim 7 is characterized in that, the coupling agent of described bifunctional is N-β-(aminoethyl)-γ-An Bingjisanjiayangjiguiwan.
9. preparation method according to claim 7 is characterized in that, the mass ratio of described soft segment of polyurethane and hard section is 1: 2.5～1: 4.
10. preparation method according to claim 7 is characterized in that, described ketoxime is a Diacetylmonoxime.
11. the application of described antibiotic Waterproof Breathable composite functional material aspect fabric, it is characterized in that, select ketoxime organic micromolecule for use with active-H group, polyurethane/nano antimicrobial particle mixture performed polymer is carried out end capping, and when fabric carried out coating, attemperation is with end capped isocyanic ester deblocking, generate the carboxylamine ester structure with the hydroxyl-OH reaction on the fabric, generate chemical bond and reach firm adhesive effect between polyurethane/nano antimicrobial particle mixture and fabric, its chemical equation is as follows:
12. the application of described antibiotic Waterproof Breathable composite functional material in the preparation medical protective garment.
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| CN105694438A (en) * | 2016-02-18 | 2016-06-22 | 惠州市环美盛新材料有限公司 | Nano inorganic antibacterial fiber masterbatch and preparation method thereof |
| CN106220806A (en) * | 2016-07-26 | 2016-12-14 | 福建师范大学泉港石化研究院 | A kind of antibacterial thermoplastic polyurethane and preparation method thereof |
| CN107829213A (en) * | 2017-12-08 | 2018-03-23 | 天津工业大学 | A kind of antibacterial Waterproof Breathable nano fibrous membrane and preparation method thereof |
| CN111909356A (en) * | 2020-08-24 | 2020-11-10 | 温州大学新材料与产业技术研究院 | Medical polyurethane material and preparation method thereof |
| CN114311861A (en) * | 2021-12-28 | 2022-04-12 | 浙江东进新材料有限公司 | Waterproof and antibacterial composite functional fabric |
| CN115012093A (en) * | 2022-07-05 | 2022-09-06 | 晋江康邦拓新材料科技有限公司 | Antibacterial and water-repellent fabric and processing method thereof |
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