CN103130957A - 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 the medical auxiliary apparatus technical field, be specifically related to a kind of situ aggregation method and prepare the method that fabric is used Polymer/nano ZnO complex antimicrobials.
Background technology
Inevitably can touch the microorganisms such as various bacteriums, fungi in life, these microorganisms can breed rapidly, and spread disease by modes such as contacts under suitable ambient conditions, affect people's healthy and normal work, studying and living.Fiber belongs to porous material, can form the polylayer forest in countless spaces again after the stack braiding, so fabric is easier to adsorb mushroom.Antibacterial finish is exactly to make fabric have the function that suppresses fungus grown, keeps the clothing living environment of health, guarantees HUMAN HEALTH, and therefore, fabric has become one of very important means of added value that improve textiles with antibacterial finishing agent.
Along with going deep into of development in science and technology research, the research of nanotechnology and application become 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 antibiotic, and the investigator is applied in textile finishing, has certain germ resistance.
In order to give fabric more excellent performance, many investigators are applied to nano zine oxide and the compound preparation nano composite material of organism in antibiotic finish of the fabric.The nano composite material for preparing in-situ method can improve consistency and the dispersiveness of nanoparticle and polymeric matrix, and the primary formation and the state that have kept nanoparticle, the various groups that can make again nanoparticle surface fully with polymer molecule generation physics or chemical action, by interface interactions different between nanoparticle and polymeric matrix, the performance of matrix polymer is produced different impacts.
Summary of the invention
The purpose of this invention is to provide the situ aggregation method that a kind ofly is applied to Cotton Fabric, the antibacterial fabric rate is high and has simultaneously certain uvioresistant performance and prepare fabric with the method for Polymer/nano ZnO complex antimicrobials.
The technical solution adopted in the present invention is:
Situ aggregation method prepares the method that fabric is used Polymer/nano ZnO complex antimicrobials, it is characterized in that:
Realized by following steps:
Step 1: get the 0.15-0.75g nano zine oxide in 30g water, utilize the ultrasonic 30min of ultrasonic grinder, make the nano zine oxide aqueous dispersion;
Step 2: the 2.4-4.8g initiator is dissolved in 15-20g water, is mixed with initiator solution;
Step 3: with 250ml there-necked flask heating in water bath to 75-90 ℃, stirrer begins to stir, open water of condensation, adding successively while stirring the 90-105g massfraction is 2/3 of the initiator solution total amount for preparing in the silane coupling agent, step 2 of the ultrasonic good nano zine oxide aqueous solution, 0.075-0.375g in 60% the dimethyl diallyl ammonium chloride aqueous solution, step 1, stirring reaction 8-15min;
Add again 1/6 of the initiator solution total amount for preparing in 0.4-1.5g glycidyl allyl ether and step 2, stirring reaction 10-20min;
Add 1/6 of the initiator solution total amount for preparing in 0.5-1.5g glycidyl allyl ether and step 2, insulated and stirred reaction 3.5h-5.0h is down to room temperature again, regulate pH to 3.7-5.0, stop stirring, close water of condensation, namely get fabric Polymer/nano ZnO matrix material.
In step 1, 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 is chosen the hydrochloric acid soln that volumetric molar concentration is 1mol/L.
The present invention has the following advantages:
The present invention is take dimethyl diallyl ammonium chloride, glycidyl allyl ether, nano-ZnO, double bond containing silane coupling agent as raw material, adopt double bond containing Nano-zinc Oxide by Silane Coupling Agents to carry out chemical modification, and then prepare the Polymer/nano zinc oxide composite with double bond containing monomer by radical polymerization, be applied to textile finishing, has good germ resistance, antibiotic rate reaches more than 95%, gives simultaneously fabric certain uvioresistant performance.
Embodiment
The present invention will be described in detail below in conjunction with embodiment.
Situ aggregation method involved in the present invention prepares the method that fabric is used Polymer/nano ZnO complex antimicrobials, is realized by following steps:
Step 1: get the 0.15-0.75g nano zine oxide in 30g water, utilize the ultrasonic 30min of ultrasonic grinder, make the nano zine oxide aqueous dispersion;
Wherein, the ultrasonic power of ultrasonic grinder is 400-800W.
Step 2: the 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: with 250ml there-necked flask heating in water bath to 75-90 ℃, stirrer begins to stir, open water of condensation, adding successively while stirring the 90-105g massfraction is 2/3 of the initiator solution total amount for preparing in the silane coupling agent, step 2 of the ultrasonic good nano zine oxide aqueous solution, 0.075-0.375g in 60% the dimethyl diallyl ammonium chloride aqueous solution, step 1, stirring reaction 8-15min;
Add again 1/6 of the initiator solution total amount for preparing in 0.4-1.5g glycidyl allyl ether and step 2, stirring reaction 10-20min;
Add 1/6 of the initiator solution total amount for preparing in 0.5-1.5g glycidyl allyl ether and step 2, insulated and stirred reaction 3.5h-5.0h is down to room temperature again, regulate pH to 3.7-5.0, stop stirring, close water of condensation, namely get 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 is chosen the hydrochloric acid soln that volumetric molar concentration is 1mol/L.
Embodiment 1:
Step 1: get the 0.15g nano zine oxide in 30g water, utilize the ultrasonic 30min of ultrasonic grinder, make the nano zine oxide aqueous dispersion;
Wherein, the ultrasonic power of ultrasonic grinder is 400W.
Step 2: the 2.4g initiator is dissolved in 15g water, is mixed with initiator solution;
Wherein, initiator is chosen Potassium Persulphate.
Step 3: with 250ml there-necked flask heating in water bath to 75 ℃, stirrer begins to stir, open water of condensation, adding successively while stirring the 90g massfraction is 2/3 of the initiator solution total amount for preparing in the silane coupling agent, step 2 of the ultrasonic good nano zine oxide aqueous solution, 0.075g in 60% the dimethyl diallyl ammonium chloride aqueous solution, step 1, stirring reaction 8min;
Add again 1/6 of the initiator solution total amount for preparing in 0.4g glycidyl allyl ether and step 2, stirring reaction 10min;
Add 1/6 of the initiator solution total amount for preparing in 0.5g glycidyl allyl ether and step 2, insulated and stirred reaction 3.5h is down to room temperature, regulates pH to 3.7, stops stirring, and closes water of condensation again, namely gets fabric with Polymer/nano ZnO matrix material;
Wherein, the stirring velocity of stirrer is 300rpm;
Silane coupling agent is chosen A-151;
PH adjusting agent is chosen the hydrochloric acid soln that volumetric molar concentration is 1mol/L.
Embodiment 2:
Step 1: get the 0.45g nano zine oxide in 30g water, utilize the ultrasonic 30min of ultrasonic grinder, make the nano zine oxide aqueous dispersion;
Wherein, the ultrasonic power of ultrasonic grinder is 600W.
Step 2: the 3.6g initiator is dissolved in 18g water, is mixed with initiator solution;
Wherein, initiator is chosen Potassium Persulphate.
Step 3: with 250ml there-necked flask heating in water bath to 80 ℃, stirrer begins to stir, open water of condensation, adding successively while stirring the 100g massfraction is 2/3 of the initiator solution total amount for preparing in the silane coupling agent, step 2 of the ultrasonic good nano zine oxide aqueous solution, 0.225g in 60% the dimethyl diallyl ammonium chloride aqueous solution, step 1, stirring reaction 12min;
Add again 1/6 of the initiator solution total amount for preparing in 0.9g glycidyl allyl ether and step 2, stirring reaction 15min;
Add 1/6 of the initiator solution total amount for preparing in 1g glycidyl allyl ether and step 2, insulated and stirred reaction 4h is down to room temperature, regulates pH to 4.3, stops stirring, and closes water of condensation again, namely gets fabric with Polymer/nano ZnO matrix material;
Wherein, the stirring velocity of stirrer is 400rpm;
Silane coupling agent is chosen A-151;
PH adjusting agent is chosen the hydrochloric acid soln that volumetric molar concentration is 1mol/L.
Embodiment 3:
Step 1: get the 0.75g nano zine oxide in 30g water, utilize the ultrasonic 30min of ultrasonic grinder, make the nano zine oxide aqueous dispersion;
Wherein, the ultrasonic power of ultrasonic grinder is 800W.
Step 2: the 4.8g initiator is dissolved in 20g water, is mixed with initiator solution;
Wherein, initiator is chosen ammonium persulphate.
Step 3: with 250ml there-necked flask heating in water bath to 90 ℃, stirrer begins to stir, open water of condensation, adding successively while stirring the 105g massfraction is 2/3 of the initiator solution total amount for preparing in the silane coupling agent, step 2 of the ultrasonic good nano zine oxide aqueous solution, 0.375g in 60% the dimethyl diallyl ammonium chloride aqueous solution, step 1, stirring reaction 15min;
Add again 1/6 of the initiator solution total amount for preparing in 1.5g glycidyl allyl ether and step 2, stirring reaction 20min;
Add 1/6 of the initiator solution total amount for preparing in 1.5g glycidyl allyl ether and step 2, insulated and stirred reaction 5.0h is down to room temperature, regulates pH to 5.0, stops stirring, and closes water of condensation again, namely gets fabric with Polymer/nano ZnO matrix material;
Wherein, the stirring velocity of stirrer is 500rpm;
Silane coupling agent is chosen KH-570;
PH adjusting agent is chosen the hydrochloric acid soln that volumetric molar concentration is 1mol/L.
The Polymer/nano ZnO matrix material that makes is applied in textile finishing, detects the germ resistance that does not arrange 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 blank and the arrangement cloth specimen, Performance Detection such as table 1:
Table 1 Polymer/nano ZnO matrix material is applied to performance test after textile finishing
It is cited that content of the present invention is not limited to embodiment, and the conversion of any equivalence that those of ordinary skills take technical solution of the present invention by reading specification sheets of the present invention is claim of the present invention and contains.
Claims (6)
1. situ aggregation method prepares the method that fabric is used Polymer/nano ZnO complex antimicrobials, it is characterized in that:
Realized by following steps:
Step 1: get the 0.15-0.75g nano zine oxide in 30g water, utilize the ultrasonic 30min of ultrasonic grinder, make the nano zine oxide aqueous dispersion;
Step 2: the 2.4-4.8g initiator is dissolved in 15-20g water, is mixed with initiator solution;
Step 3: with 250ml there-necked flask heating in water bath to 75-90 ℃, stirrer begins to stir, open water of condensation, adding successively while stirring the 90-105g massfraction is 2/3 of the initiator solution total amount for preparing in the silane coupling agent, step 2 of the ultrasonic good nano zine oxide aqueous solution, 0.075-0.375g in 60% the dimethyl diallyl ammonium chloride aqueous solution, step 1, stirring reaction 8-15min;
Add again 1/6 of the initiator solution total amount for preparing in 0.4-1.5g glycidyl allyl ether and step 2, stirring reaction 10-20min;
Add 1/6 of the initiator solution total amount for preparing in 0.5-1.5g glycidyl allyl ether and step 2, insulated and stirred reaction 3.5h-5.0h is down to room temperature again, regulate pH to 3.7-5.0, stop stirring, close water of condensation, namely get fabric Polymer/nano ZnO matrix material.
2. situ aggregation method according to claim 1 prepares the method that fabric is used Polymer/nano ZnO complex antimicrobials, it is characterized in that:
In step 1, the ultrasonic power of ultrasonic grinder is 400-800W.
3. situ aggregation method according to claim 1 and 2 prepares the method that fabric is used 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 that fabric is used 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 that fabric is used 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 that fabric is used Polymer/nano ZnO complex antimicrobials, it is characterized in that:
In step 3, pH adjusting agent is chosen the hydrochloric acid soln that volumetric molar concentration is 1mol/L.
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CN102505450A (en) * | 2011-09-30 | 2012-06-20 | 陕西科技大学 | Quaternized zinc oxide sol as textile finishing agent and preparation method thereof |
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