CN103130957B - Method for preparing polymer/nano ZnO composite antimicrobial for textiles through in-situ polymerization method - Google Patents
Method for preparing polymer/nano ZnO composite antimicrobial for textiles through in-situ polymerization method Download PDFInfo
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Abstract
The invention relates to a method for preparing a polymer/nano ZnO composite antimicrobial for textiles through an in-situ polymerization method. The nano ZnO has the characteristics of large specific area, high surface activity, excellent thermal stability and chemical stability, ultraviolet resistance, antibacterial property and the like. The method comprises the following steps of: preparing a nano ZnO aqueous solution by using ultrasonic waves; preparing an initiator solution; adding a dimethyl diallyl ammonia chloride solution, a nano ZnO solution, a silane coupling agent and 2/3 of the initiator solution in sequence under stirring and condensing conditions, and adding allyl glycidyl ether and 1/6 of the initiator aqueous solution; then adding allyl glycidyl ether and 1/6 of the initiator aqueous solution, and preserving the heat and stirring for reaction; and adjusting the pH value to obtain a composite material. According to the method, the silane coupling agent containing double bonds is adopted to perform chemical modification on the nano ZnO, and then the nano ZnO and a monomer containing double bonds are subjected to free radical polymerization to prepare the polymer/nano ZnO composite material. If the composite material is applied to textile dressing, the antibacterial rate reaches over 95%, and textiles are endowed with a certain ultraviolent resistance.
Description
Technical field
the invention belongs to antibacterial fabric processing technology field, be specifically related to a kind of method that situ aggregation method prepares fabric Polymer/nano ZnO complex antimicrobials.
Background technology
Inevitably touch the microorganisms such as various bacterium, fungi in life, these microorganisms, under suitable ambient conditions, can breed rapidly, and are spread disease by modes such as contacts, affect the healthy of people and normal work, studying and living.Fiber belongs to porous material, can form again the polylayer forest in countless space after superposition braiding, and therefore fabric is easier to adsorb mushroom.Antibacterial finish is exactly make fabric have the function suppressing fungus grown, maintains the clothing living environment of health, ensures HUMAN HEALTH, and therefore, fabric antibacterial finishing agent has become one of very important means of added value improving textiles.
Along with going deep into of development in science and technology research, the Study and appliance of nanotechnology becomes focus gradually.Nano zine oxide has that specific surface area is large, surfactivity is high, thermostability and chemical stability is good, uvioresistant and the characteristic such as antibacterial, and investigator is applied in textile finishing, has certain germ resistance.
In order to give fabric more excellent performance, nano zine oxide and organism compound are prepared nano composite material by many investigators, are applied in antibiotic finish of the fabric.Nano composite material of preparing in-situ method can improve consistency and the dispersiveness of nanoparticle and polymeric matrix, and maintain primary formation and the state of nanoparticle, the various groups that can make again nanoparticle surface fully with polymer molecule generation physics or chemical action, produce different impacts by the performance of interface interactions different between nanoparticle from polymeric matrix on matrix polymer.
Summary of the invention
The object of this invention is to provide a kind of method being applied to the high and situ aggregation method simultaneously with certain uvioresistant performance of Cotton Fabric, antibacterial fabric rate and preparing fabric Polymer/nano ZnO complex antimicrobials.
The technical solution adopted in the present invention is:
Situ aggregation method prepares the method for fabric Polymer/nano ZnO complex antimicrobials, it is characterized in that:
Realized by following steps:
Step one: get 0.15-0.75g nano zine oxide in 30g water, utilizes the ultrasonic 30min of ultrasonic grinder, obtained nano zine oxide aqueous dispersion;
Step 2: 2.4-4.8g initiator is dissolved in 15-20g water, is mixed with initiator solution;
Step 3: by 250ml there-necked flask heating in water bath to 75-90 DEG C, stirrer starts to stir, open water of condensation, add successively while stirring 90-105g massfraction be 60% the dimethyl diallyl ammonium chloride aqueous solution, prepare in the silane coupling agent of the ultrasonic good nano zine oxide aqueous solution, 0.075-0.375g, step 2 in step one 2/3, stirring reaction 8-15min of initiator solution total amount;
Add 1/6 of the initiator solution total amount prepared in 0.4-1.5g glycidyl allyl ether and step 2, stirring reaction 10-20min again;
Add 1/6 of the initiator solution total amount prepared in 0.5-1.5g glycidyl allyl ether and step 2 again, insulated and stirred reaction 3.5h-5.0h, is down to room temperature, regulate pH to 3.7-5.0, stop stirring, close water of condensation, obtain fabric Polymer/nano ZnO matrix material.
In step one, the ultrasonic power of ultrasonic grinder is 400-800W.
In step 2, initiator is selected from Potassium Persulphate, ammonium persulphate.
In step 3, the stirring velocity of stirrer is 300rpm-500rpm.
In step 3, silane coupling agent is selected from A-151, KH-570.
In step 3, pH adjusting agent chooses the hydrochloric acid soln that volumetric molar concentration is 1mol/L.
The present invention has the following advantages:
The present invention with dimethyl diallyl ammonium chloride, glycidyl allyl ether, nano-ZnO, double bond containing silane coupling agent for raw material, double bond containing Nano-zinc Oxide by Silane Coupling Agents is adopted to carry out chemical modification, and then prepare Polymer/nano zinc oxide composite with double bond containing monomer by radical polymerization, be applied to textile finishing, there is good germ resistance, antibiotic rate reaches more than 95%, gives fabric certain uvioresistant performance simultaneously.
Embodiment
Below in conjunction with embodiment, the present invention will be described in detail.
Situ aggregation method involved in the present invention prepares the method for fabric Polymer/nano ZnO complex antimicrobials, is realized by following steps:
Step one: get 0.15-0.75g nano zine oxide in 30g water, utilizes the ultrasonic 30min of ultrasonic grinder, obtained nano zine oxide aqueous dispersion;
Wherein, the ultrasonic power of ultrasonic grinder is 400-800W.
Step 2: 2.4-4.8g initiator is dissolved in 15-20g water, is mixed with initiator solution;
Wherein, initiator is selected from Potassium Persulphate, ammonium persulphate.
Step 3: by 250ml there-necked flask heating in water bath to 75-90 DEG C, stirrer starts to stir, open water of condensation, add successively while stirring 90-105g massfraction be 60% the dimethyl diallyl ammonium chloride aqueous solution, prepare in the silane coupling agent of the ultrasonic good nano zine oxide aqueous solution, 0.075-0.375g, step 2 in step one 2/3, stirring reaction 8-15min of initiator solution total amount;
Add 1/6 of the initiator solution total amount prepared in 0.4-1.5g glycidyl allyl ether and step 2, stirring reaction 10-20min again;
Add 1/6 of the initiator solution total amount prepared in 0.5-1.5g glycidyl allyl ether and step 2 again, insulated and stirred reaction 3.5h-5.0h, is down to room temperature, regulate pH to 3.7-5.0, stop stirring, close water of condensation, obtain fabric Polymer/nano ZnO matrix material;
Wherein, the stirring velocity of stirrer is 300rpm-500rpm;
Silane coupling agent is selected from A-151, KH-570;
PH adjusting agent chooses the hydrochloric acid soln that volumetric molar concentration is 1mol/L.
Embodiment 1:
Step one: get 0.15g nano zine oxide in 30g water, utilizes the ultrasonic 30min of ultrasonic grinder, obtained nano zine oxide aqueous dispersion;
Wherein, the ultrasonic power of ultrasonic grinder is 400W.
Step 2: 2.4g initiator is dissolved in 15g water, is mixed with initiator solution;
Wherein, Potassium Persulphate chosen by initiator.
Step 3: by 250ml there-necked flask heating in water bath to 75 DEG C, stirrer starts to stir, open water of condensation, add successively while stirring 90g massfraction be 60% the dimethyl diallyl ammonium chloride aqueous solution, prepare in the silane coupling agent of the ultrasonic good nano zine oxide aqueous solution, 0.075g, step 2 in step one 2/3, stirring reaction 8min of initiator solution total amount;
Add 1/6 of the initiator solution total amount prepared in 0.4g glycidyl allyl ether and step 2, stirring reaction 10min again;
Add 1/6 of the initiator solution total amount prepared in 0.5g glycidyl allyl ether and step 2 again, insulated and stirred reaction 3.5h, is down to room temperature, regulates pH to 3.7, stops stirring, closes water of condensation, obtain fabric Polymer/nano ZnO matrix material;
Wherein, the stirring velocity of stirrer is 300rpm;
Silane coupling agent chooses A-151;
PH adjusting agent chooses the hydrochloric acid soln that volumetric molar concentration is 1mol/L.
Embodiment 2:
Step one: get 0.45g nano zine oxide in 30g water, utilizes the ultrasonic 30min of ultrasonic grinder, obtained nano zine oxide aqueous dispersion;
Wherein, the ultrasonic power of ultrasonic grinder is 600W.
Step 2: 3.6g initiator is dissolved in 18g water, is mixed with initiator solution;
Wherein, Potassium Persulphate chosen by initiator.
Step 3: by 250ml there-necked flask heating in water bath to 80 DEG C, stirrer starts to stir, open water of condensation, add successively while stirring 100g massfraction be 60% the dimethyl diallyl ammonium chloride aqueous solution, prepare in the silane coupling agent of the ultrasonic good nano zine oxide aqueous solution, 0.225g, step 2 in step one 2/3, stirring reaction 12min of initiator solution total amount;
Add 1/6 of the initiator solution total amount prepared in 0.9g glycidyl allyl ether and step 2, stirring reaction 15min again;
Add 1/6 of the initiator solution total amount prepared in 1g glycidyl allyl ether and step 2 again, insulated and stirred reaction 4h, is down to room temperature, regulates pH to 4.3, stops stirring, closes water of condensation, obtain fabric Polymer/nano ZnO matrix material;
Wherein, the stirring velocity of stirrer is 400rpm;
Silane coupling agent chooses A-151;
PH adjusting agent chooses the hydrochloric acid soln that volumetric molar concentration is 1mol/L.
Embodiment 3:
Step one: get 0.75g nano zine oxide in 30g water, utilizes the ultrasonic 30min of ultrasonic grinder, obtained nano zine oxide aqueous dispersion;
Wherein, the ultrasonic power of ultrasonic grinder is 800W.
Step 2: 4.8g initiator is dissolved in 20g water, is mixed with initiator solution;
Wherein, ammonium persulphate chosen by initiator.
Step 3: by 250ml there-necked flask heating in water bath to 90 DEG C, stirrer starts to stir, open water of condensation, add successively while stirring 105g massfraction be 60% the dimethyl diallyl ammonium chloride aqueous solution, prepare in the silane coupling agent of the ultrasonic good nano zine oxide aqueous solution, 0.375g, step 2 in step one 2/3, stirring reaction 15min of initiator solution total amount;
Add 1/6 of the initiator solution total amount prepared in 1.5g glycidyl allyl ether and step 2, stirring reaction 20min again;
Add 1/6 of the initiator solution total amount prepared in 1.5g glycidyl allyl ether and step 2 again, insulated and stirred reaction 5.0h, is down to room temperature, regulates pH to 5.0, stops stirring, closes water of condensation, obtain fabric Polymer/nano ZnO matrix material;
Wherein, the stirring velocity of stirrer is 500rpm;
Silane coupling agent chooses KH-570;
PH adjusting agent chooses the hydrochloric acid soln that volumetric molar concentration is 1mol/L.
Obtained Polymer/nano ZnO matrix material is applied in textile finishing, detects the germ resistance not arranging cloth specimen and arrange rear cloth specimen according to succusion in " FZ/T 73023-2006 antibiosis knitting product "; To not arrange cloth specimen as blank, detect ultraviolet permeability that is blank and arrangement cloth specimen, Performance Detection is as table 1:
Table 1 Polymer/nano ZnO matrix material is applied to performance test after textile finishing
Content of the present invention is not limited to cited by embodiment, and the conversion of those of ordinary skill in the art by reading specification sheets of the present invention to any equivalence that technical solution of the present invention is taked, is claim of the present invention and contains.
Claims (6)
1. situ aggregation method prepares the method for fabric Polymer/nano ZnO complex antimicrobials, it is characterized in that:
Realized by following steps:
Step one: get 0.15-0.75g nano zine oxide in 30g water, utilizes the ultrasonic 30min of ultrasonic grinder, obtained nano zine oxide aqueous dispersion;
Step 2: 2.4-4.8g initiator is dissolved in 15-20g water, is mixed with initiator solution;
Step 3: by 250ml there-necked flask heating in water bath to 75-90 DEG C, stirrer starts to stir, open water of condensation, add successively while stirring 90-105g massfraction be 60% the dimethyl diallyl ammonium chloride aqueous solution, prepare in the silane coupling agent of the ultrasonic good nano zine oxide aqueous solution, 0.075-0.375g, step 2 in step one 2/3, stirring reaction 8-15min of initiator solution total amount;
Add 1/6 of the initiator solution total amount prepared in 0.4-1.5g glycidyl allyl ether and step 2, stirring reaction 10-20min again;
Add 1/6 of the initiator solution total amount prepared in 0.5-1.5g glycidyl allyl ether and step 2 again, insulated and stirred reaction 3.5h-5.0h, is down to room temperature, regulate pH to 3.7-5.0, stop stirring, close water of condensation, obtain fabric Polymer/nano ZnO matrix material.
2. situ aggregation method according to claim 1 prepares the method for fabric Polymer/nano ZnO complex antimicrobials, it is characterized in that:
In step one, the ultrasonic power of ultrasonic grinder is 400-800W.
3. situ aggregation method according to claim 1 and 2 prepares the method for fabric Polymer/nano ZnO complex antimicrobials, it is characterized in that:
In step 2, initiator is selected from Potassium Persulphate, ammonium persulphate.
4. situ aggregation method according to claim 3 prepares the method for fabric Polymer/nano ZnO complex antimicrobials, it is characterized in that:
In step 3, the stirring velocity of stirrer is 300rpm-500rpm.
5. situ aggregation method according to claim 4 prepares the method for fabric Polymer/nano ZnO complex antimicrobials, it is characterized in that:
In step 3, silane coupling agent is selected from A-151, KH-570.
6. situ aggregation method according to claim 5 prepares the method for fabric Polymer/nano ZnO complex antimicrobials, it is characterized in that:
In step 3, pH adjusting agent chooses the hydrochloric acid soln that volumetric molar concentration is 1mol/L.
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| CN104862967B (en) * | 2014-02-24 | 2017-05-24 | 香港纺织及成衣研发中心有限公司 | Fabric with surface cooling function and preparation method thereof |
| CN104650290B (en) * | 2015-02-05 | 2017-07-18 | 陕西科技大学 | Use for synthetic leather polymer nanocomposite ZnO complex antimicrobials based on situ aggregation method and preparation method thereof |
| CN104892828A (en) * | 2015-05-25 | 2015-09-09 | 陕西科技大学 | Method for preparing polyacrylate/nano ZnO composite leather finishing agent by Pickering emulsion polymerization |
| TWI581714B (en) * | 2016-01-04 | 2017-05-11 | 台虹科技股份有限公司 | Antibacterial deodorant powder, antibacterial deodorant masterbatch and antibacterial deodorant structure |
| CN105648745B (en) * | 2016-04-01 | 2018-04-17 | 陕西科技大学 | Fabric polymer matrix cerium-doped nanometer zinc oxide composite antibiosis agent and preparation method thereof |
| CN106381039A (en) * | 2016-08-22 | 2017-02-08 | 浙江西大门新材料股份有限公司 | Antibacterial curtain and preparation method thereof |
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| CN106555329B (en) * | 2016-10-21 | 2019-04-16 | 上海纳米技术及应用国家工程研究中心有限公司 | A method of antibacterial dacron is prepared with ultrasonic radiation method |
| CN107287900B (en) * | 2017-07-20 | 2019-08-13 | 科凯精细化工（上海）有限公司 | The preparation method of composite antibacterial finishing agent |
| CN107401051B (en) * | 2017-07-20 | 2019-11-15 | 科凯精细化工（上海）有限公司 | Zinc oxide-QAS polymer complex antimicrobials and preparation method thereof |
| CN107287899B (en) * | 2017-07-20 | 2019-08-13 | 科凯精细化工（上海）有限公司 | The antibiotic finishing method of cotton fabric |
| CN109517121B (en) * | 2018-11-01 | 2021-03-23 | 陕西科技大学 | Organosilicon quaternary ammonium salt/(Ag/ZnO) nano antibacterial agent and preparation method and application thereof |
| CN109487536B (en) * | 2018-11-01 | 2021-07-27 | 陕西科技大学 | Epoxy group-containing organosilicon quaternary ammonium salt/(zinc oxide @ carbon quantum dot) nano composite antibacterial agent and preparation method and application thereof |
| CN113638226B (en) * | 2021-09-17 | 2024-04-02 | 四川华纺银华有限责任公司 | Finishing method of antibacterial fiber, fiber and textile thereof |
| CN113981680B (en) * | 2021-11-16 | 2023-12-26 | 青岛大学 | Washable antibacterial fabric and preparation method thereof |
| CN115161993A (en) * | 2022-05-25 | 2022-10-11 | 浙江理工大学 | Organic/inorganic bonding type composite antibacterial agent, preparation method and application thereof |
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| CN102505450B (en) * | 2011-09-30 | 2013-06-19 | 陕西科技大学 | Quaternized zinc oxide sol as textile finishing agent and preparation method thereof |
| CN102787497B (en) * | 2012-09-05 | 2014-05-14 | 陕西科技大学 | Method for preparing novel quaternary ammonium salt copolymer/nanometer ZnO composite antimicrobial for fabric |
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