CN112127209B - Method for in-situ reduction loading of nano silver particles on surface of cellulose paper - Google Patents
Method for in-situ reduction loading of nano silver particles on surface of cellulose paper Download PDFInfo
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- CN112127209B CN112127209B CN202010946649.8A CN202010946649A CN112127209B CN 112127209 B CN112127209 B CN 112127209B CN 202010946649 A CN202010946649 A CN 202010946649A CN 112127209 B CN112127209 B CN 112127209B
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H25/00—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00
- D21H25/04—Physical treatment, e.g. heating, irradiating
- D21H25/06—Physical treatment, e.g. heating, irradiating of impregnated or coated paper
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H25/00—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00
- D21H25/02—Chemical or biochemical treatment
Abstract
The application provides a method for carrying nano silver particles on the surface of cellulose paper by in-situ reduction, which comprises the following steps: pretreating cellulose paper by using an alkaline solution; and atomizing the silver source solution by adopting an ultrasonic atomizer, applying voltage to the atomized fog drops by using a high-voltage direct-current power supply to induce the atomized fog drops to be charged, leading the charged atomized fog drops to the surface of the cellulose paper, and loading nano silver particles on the surface of the cellulose paper in situ. The method provided by the invention has mild experimental reaction conditions, is green and environment-friendly, the prepared nano silver particles have narrow particle size distribution and good loading stability, and the agglomeration phenomenon caused by high surface energy when the nano silver particles are loaded on the surface of cellulose paper can be effectively solved, so that the function of the nano silver particles can be better exerted.
Description
Technical Field
The application relates to the field of paper surface treatment, in particular to a method for carrying nano silver particles on the surface of cellulose paper through in-situ reduction.
Background
At present, paper used by people is basically composed of cellulose, each basic ring in a cellulose molecular chain has three alcoholic hydroxyl groups, and each cellulose macromolecular chain also has two terminal hydroxyl groups, wherein C1The glycoside hydroxyl group at the position is a reducing end group, and the other end is C4The hydroxyl group in position is a non-reducing end group. Due to the existence of the groups, cellulose molecules have certain reactivity, but after the cellulose molecular chains form the paper, many active groups on the surface of the paper cannot be exposed due to the existence of hydrogen bonds and other acting forces, so that the surface of the paper is inert as a whole.
Silver is an ancient bacteriostatic material and has been used for more than two thousand years with respect to its antimicrobial properties. Recently, with the development of science and technology, people begin to utilize nano silver as a new antibacterial material. The nano silver and silver ions are the same, and can be adsorbed on the surface of a cell membrane to destroy the cell membrane and penetrate into the interior of a bacterial cell, so that the cell permeation and the respiratory function are influenced. Compared with the traditional silver ions, the nano silver has large specific surface area, is not easy to be oxidized and precipitated, and can better play an antibacterial role.
However, the silver nanoparticles are unstable due to their high specific surface energy, and are easily agglomerated, so that a dispersant, a stabilizer, a carrier, and the like are often used in the preparation and use processes thereof. Due to the nature of the nano silver particles, the aggregation is easy to occur when the nano silver particles are loaded on the surface of the cellulose paper.
Disclosure of Invention
Based on the above, it is necessary to provide a method for reducing and loading silver nanoparticles on the surface of cellulose paper in situ, aiming at the technical problem that the silver nanoparticles are easy to agglomerate when loaded on the surface of the cellulose paper.
A method for carrying nano silver particles on the surface of cellulose paper by in-situ reduction comprises the following steps:
pretreating cellulose paper by using an alkaline solution;
and atomizing the silver source solution by adopting an ultrasonic atomizer, applying voltage to the atomized fog drops by using a high-voltage direct-current power supply to induce the atomized fog drops to be charged, leading the charged atomized fog drops to the surface of the cellulose paper, and loading nano silver particles on the surface of the cellulose paper in situ.
In the technical scheme, firstly, the cellulose paper is pretreated by adopting an alkaline solution, and the alkaline solution can activate the cellulose on the surface of the paper and remove the hydrogen bond effect, so that more active groups are liberated, and the reactivity of the surface of the cellulose paper is enhanced. Secondly, ultrasonic atomization is a method for dispersing a solution into tiny droplets by utilizing ultrasonic waves, the particle size of the droplets generated by ultrasonic atomization is about 5-10 microns, and reactive substances in the solution can be effectively and uniformly dispersed in the droplets. The high-voltage direct-current power supply applies voltage to the atomized fog drops, namely the high voltage is applied after the liquid solution is atomized, so that the atomized fog drops carry charges, the atomized fog drops are broken into smaller fog drops under the action of an electric field force, the ultrasonic atomization and the electrostatic high voltage are combined to be used for in-situ preparation of the nano silver particles on cellulose paper, the agglomeration of the nano silver particles can be reduced, and the loading capacity and the load firmness of the nano silver particles are increased.
Several alternatives are provided below, but not as an additional limitation to the above general solution, but merely as a further addition or preference, each alternative being combinable individually for the above general solution or among several alternatives without technical or logical contradictions.
Optionally, the method for in-situ reduction loading of nano silver particles on the surface of cellulose paper comprises the following steps: the cellulose sheet is treated in cold plasma. The order of pretreatment of the cellulose sheet with an alkaline solution or treatment in cold plasma can be reversed.
Optionally, the method for in-situ reduction loading of nano silver particles on the surface of cellulose paper comprises the following steps:
1) pretreating cellulose paper by using an alkaline solution;
2) treating the cellulose paper in cold plasma;
3) the silver source solution is atomized by an ultrasonic atomizer, voltage is applied to atomized fog drops by a high-voltage direct-current power supply to enable the atomized fog drops to be inductively charged, the charged atomized fog drops are led to the surface of the cellulose paper, and nano silver particles are loaded on the surface of the cellulose paper in situ.
In the step 2), the surface of the cellulose paper treated by the alkaline solution is subjected to cold plasma treatment, and water molecules and oxygen molecules in the air are excited under the action of an electric field to generate H2O+,O2 +，O2 +(H2O), and the like, which are further ionized under the action of an electric field to finally generate hydroxyl radicals, and then the hydroxyl radicals are attached to the surface of the paper under the action of the electric field, so that the agglomeration of the nano silver particles can be further reduced, and the loading capacity and the loading firmness of the nano silver particles can be increased.
Optionally, the cellulose paper is selected from various common machine-made papers, handsheets and specialty functional papers, including: one or more of qualitative filter paper, newsprint, printing paper, dictionary paper, rice paper and the like.
Optionally, the pretreatment method includes: the cellulose paper is soaked in an alkaline solution or sprayed on the surface of the cellulose paper by the alkaline solution.
Further preferably, the pretreatment mode is that the cellulose paper is soaked in an alkaline solution, and the soaking time of the cellulose paper in the alkaline solution is 0.5-5 min.
Further preferably, the pretreatment mode adopts alkaline solution to spray on the surface of the cellulose paper, the atomization mode is ultrasonic atomization, and the atomization treatment time is 1-2 min.
Optionally, the alkaline solution comprises an inorganic alkaline solution or an organic alkaline solution. The inorganic alkaline solution is preferably a hydroxide solution of group I or II elements such as sodium hydroxide or calcium hydroxide.
Optionally, the alkaline solution is a sodium hydroxide solution or a calcium hydroxide solution.
The concentration of the alkaline solution used for treating the cellulose sheet is not excessively high in view of the fact that the alkaline solution has the effect of decomposing and destroying the structure of the cellulose sheet while activating the cellulose sheet, and preferably, the concentration of the alkaline solution should be less than 1 mol/L. But the activation effect of the alkaline solution with too low concentration on the cellulose paper is relatively limited, and optionally, the concentration of the alkaline solution is 0.05-0.2 mol/L.
The nano silver particles are dispersed and loaded on the cellulose paper in situ, the selection of the silver source solution can also influence the loading effect of the final nano silver particles, and preferably, the silver source solution is silver nitrate solution or silver ammonia solution.
The silver source solution subjected to ultrasonic atomization is used as a source for loading nano silver particles on the surface of the cellulose paper, and the concentration of the silver source solution subjected to ultrasonic atomization cannot be too large or too small in consideration of the particle size of nano silver finally loaded on the cellulose paper, preferably the concentration of the silver source solution is 5-60 mmol/L, and further preferably the concentration of the silver source solution is 10-50 mmol/L.
The action time of the cellulose paper and fog drops generated by atomization of the silver source solution needs to be controlled within a certain range, the action time is too short, the nano silver particles cannot be uniformly dispersed and loaded on the cellulose paper, the action time is too long, the nano silver particles are easy to agglomerate, the loading effect of the nano silver particles is influenced, and preferably, the time for the cellulose paper to contact with the ultrasonic atomization fog drops is 1-5 min.
The atomized fog drops are applied with voltage through a high-voltage direct-current power supply, the atomized fog drops generated by ultrasonic atomization can be inductively charged due to the introduction of an electrostatic voltage environment, the degree of inductive charging of the atomized fog drops mainly depends on the value of the applied external voltage, and the voltage applied to the atomized fog drops is preferably 5-25 kV. When the voltage is lower, the inductive electrification degree of the atomized fog drops is not obvious, when the voltage value exceeds 20kV, air near the high-voltage output end is ionized, the electrification process of the atomized fog drops is converted into the mixed action of inductive electrification and contact electrification, the charge distribution uniformity of the fog drops is reduced, and therefore the voltage applied to the atomized fog drops is further preferably 10-20 kV.
Optionally, the discharge mode of the cold plasma is dielectric barrier discharge, and the atmosphere is air or a mixed gas of hydrogen and argon.
Optionally, the voltage is 50-100V and the current is 0.2-0.5A in the cold plasma treatment process. Further preferably, the voltage adjustment range is 70-80V, and the current adjustment range is 0.3-0.4A.
Optionally, the time of the cold plasma treatment is 20-60 s, and more preferably, the time is 30-40 s.
The invention has the following beneficial effects:
(1) the method utilizes the alkaline solution and the cold plasma to treat and activate the cellulose paper, does not influence the cellulose paper per se, and can obviously improve the reactivity of the surface of the cellulose paper.
(2) The invention utilizes the ultrasonic atomization method to disperse the silver source solution on the cellulose paper, so that the subsequently generated nano silver particles can keep smaller particle size and less agglomeration phenomenon, and can be firmly attached on the cellulose, thereby solving the problems of difficult and unstable loading of the nano silver particles.
(3) In the process of loading the nano-silver particles by ultrasonic atomization, high-voltage static electricity is used as an auxiliary condition, so that the ultrasonically atomized fog drops are charged, the fog drops can be intensively distributed on the surface of cellulose paper due to the electrostatic attraction effect, and the loading capacity of the nano-silver particles and the utilization rate of the silver source solution can be increased.
(4) The nano silver particles loaded on the cellulose paper in situ have narrow particle size distribution and good dispersibility, and the obtained nano silver/cellulose paper composite material has good stability.
Drawings
FIG. 1 is an SEM image of the filter paper/nano silver composite materials prepared in examples 1-2 and comparative example 1;
FIG. 2 is an XRD pattern of the filter paper/nano silver composite material prepared in example 1;
FIG. 3 is a thermogravimetric analysis graph of the filter paper/nano-silver composite prepared in example 1;
FIG. 4 is a graph showing the UV-VIS absorption spectrum of the filter paper/nano-silver composite prepared in example 1;
FIG. 5 is an XPS map of the filter paper/nano silver composite prepared in example 1;
FIG. 6 is a graph showing the results of experiments on the inhibition zones of the filter paper/nano silver composite materials prepared in examples 1-2 and comparative example 1 on Escherichia coli (left) and Staphylococcus aureus (right).
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the embodiments of the present application and the accompanying drawings, and it is obvious that the described embodiments are only a part of the embodiments of the present application, 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 application.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application.
Example 1
(1) Qualitative filter paper was cut into 20mm × 20mm size, after which the filter paper material was washed clean with absolute ethanol and dried at 80 ℃ for use.
(2) Soaking the obtained filter paper material in 0.1mol/L sodium hydroxide solution for 1min, taking out, washing with deionized water, washing with absolute ethyl alcohol, and drying at 80 ℃.
(3) And (3) treating the filter paper material obtained after drying in the step (2) in a cold plasma reaction chamber for 1min, wherein the plasma is discharged by dielectric barrier gas, the atmosphere is air, the voltage is 75V, and the current is 0.3A.
(4) Adding a silver nitrate solution with the concentration of 10mmol/L into an ultrasonic atomizer, starting the ultrasonic atomizer to fully atomize the silver nitrate solution, applying a voltage of 15kV to a copper pipe to enable atomized fog drops to pass through the copper pipe, placing a filter paper material at a fog drop outlet below the copper pipe to enable the surface of the filter paper material to fully contact with the fog drops for 2min, taking out the filter paper material after the treatment is finished, washing with deionized water, and naturally drying.
An SEM image of the filter paper/nano silver composite material prepared in this embodiment is shown in fig. 1(a), and it can be seen that the obtained nano silver particles are more uniformly distributed, the loading amount is more, and the particle size distribution is intensively distributed between 50nm and 100 nm. Under the operation of the embodiment 1, the cellulose paper is activated by adopting the alkaline solution and the cold plasma treatment, and then the method of carrying out the ultrasonic atomization loading of the nano silver particles by combining the electrostatic high voltage is adopted, so that the distribution of the nano silver particles on the cellulose paper is more uniform, the loading effect is more stable, the loading capacity is more, and the particle size distribution is more concentrated.
The XRD pattern of the filter paper/nano silver composite material prepared in this example is shown in fig. 2, and it can be seen from the distribution of 2 θ angles that the prepared nano silver is in a cubic crystal form.
The thermogravimetric analysis curve of the filter paper/nano-silver composite material prepared in this example is shown in fig. 3, and it can be seen that the mass fraction of the nano-silver particles loaded in the filter paper/nano-silver composite material is about 3.04%.
The ultraviolet-visible absorption spectrum of the filter paper/nano-silver composite material prepared in the embodiment is shown in fig. 4, and it can be seen that an obvious absorption peak appears at 410nm of the absorption spectrum, which corresponds to the absorption peak of the nano-silver particles, and the success of the nano-silver particles in the filter paper material is proved.
The XPS results of the filter paper/nano silver composite material prepared in this example are shown in fig. 5, and the full spectrum shows the existence of silver element, while the high resolution XPS analysis shows that the silver element exists in the form of simple substance in the materials, namely Ag 3d 5/2 at 368.1eV and Ag 3d 3/2 at 374.1 eV.
Example 2
(1) Qualitative filter paper was cut into 20mm × 20mm size, after which the filter paper material was washed clean with absolute ethanol and dried at 80 ℃ for use.
(2) Soaking the obtained filter paper material in 0.1mol/L sodium hydroxide solution for 1min, taking out, washing with deionized water, washing with absolute ethyl alcohol, and drying at 80 ℃.
(3) Adding a silver nitrate solution with the concentration of 10mmol/L into an ultrasonic atomizer, starting the ultrasonic atomizer to fully atomize the silver nitrate solution, applying a voltage of 15kV to a copper pipe to enable atomized fog drops to pass through the copper pipe, placing a filter paper material at a fog drop outlet below the copper pipe to enable the surface of the filter paper material to fully contact with the fog drops for 2min, taking out the filter paper material after the treatment is finished, washing with deionized water, and naturally drying.
As shown in fig. 1(b), the SEM image of the filter paper/nano silver composite material prepared in this example shows that, compared to example 1, the distribution of nano silver particles is relatively dispersed due to the absence of the cold plasma treatment, and the number of supported nano silver particles is relatively small compared to example 1, and the particle size of the nano silver particles is substantially distributed between 10nm and 50 nm.
Comparative example 1
(1) Qualitative filter paper was cut into 20mm × 20mm size, after which the filter paper material was washed clean with absolute ethanol and dried at 80 ℃ for use.
(2) Adding a silver nitrate solution with the concentration of 10mmol/L into an ultrasonic atomizer, opening the ultrasonic atomizer to fully atomize the silver nitrate solution, enabling atomized fog drops to pass through a copper pipe, placing a filter paper material at a fog drop outlet below the copper pipe to fully contact the surface of the filter paper material with the fog drops for 2min, taking out the filter paper material after the treatment is finished, washing with deionized water, and naturally drying.
As shown in fig. 1(c), the SEM image of the filter paper/nano silver composite material prepared in this example shows that since the cellulose material is not activated by the alkaline solution and the plasma, the nano silver particles are hardly seen on the cellulose.
Performance test:
the results of the experiments on the inhibition ring of the filter paper/nano silver composite material prepared in examples 1-2 and comparative example 1 on escherichia coli and staphylococcus aureus are shown in fig. 6(a), (b), and (c), which indicates that the inhibition ring of the filter paper/nano silver composite material obtained in example 1 is more obvious than that of the filter paper/nano silver composite material obtained in example 2 and comparative example 1, and that the filter paper/nano silver composite material obtained in example 1 has the best antibacterial performance.
Example 3
The sodium hydroxide solution in (2) in example 1 was replaced with a calcium hydroxide solution, and the rest of the procedure was the same as in example 1.
The distribution and particle size of the nano-silver particles on the filter paper/nano-silver composite material prepared in this example are substantially the same as those in example 1.
Example 4
The silver nitrate solution ultrasonically atomized in (4) in example 1 was changed to a silver ammonia solution, and the rest of the procedure was the same as in example 1.
The filter paper/nano-silver composite material prepared by the embodiment has the advantages of low nano-silver particle content, dispersed distribution and particle size distribution of 10-100 nm.
Example 5
The concentration of the silver nitrate solution ultrasonically atomized in (4) in example 1 was adjusted to 30mmol/L, and the rest of the procedure was the same as in example 1.
The content and distribution of nano-silver particles on the filter paper/nano-silver composite material prepared in the embodiment are basically the same as those in the embodiment 1, and the particle size is basically distributed between 70 nm and 150 nm.
Example 6
The concentration of the silver nitrate solution ultrasonically atomized in (4) in example 1 was adjusted to 50mmol/L, and the rest of the procedure was the same as in example 1.
The content and distribution of nano-silver particles on the filter paper/nano-silver composite material prepared in the embodiment are basically the same as those in the embodiment 1, and the particle size is basically distributed between 100nm and 200 nm.
Example 7
The voltage applied to the copper tube in (4) in example 1 was adjusted to 10kV, and the procedure was the same as in example 1.
Compared with the filter paper/nano-silver composite material prepared in the embodiment, the content of nano-silver particles in the filter paper/nano-silver composite material prepared in the embodiment is less, the distribution of the silver particles is basically the same as that in the embodiment 1, and the particle size is basically distributed between 30 nm and 100 nm.
Example 8
The voltage applied to the copper tube in (4) in example 1 was adjusted to 20kV, and the procedure was the same as in example 1.
The content and distribution of nano-silver particles on the filter paper/nano-silver composite material prepared in the embodiment are basically the same as those in the embodiment 1, and the particle size is basically distributed between 100nm and 300 nm.
Example 9
(1) Qualitative filter paper was cut into 20mm × 20mm size, after which the filter paper material was washed clean with absolute ethanol and dried at 80 ℃ for use.
(2) Atomizing 0.05mol/L calcium hydroxide solution with an atomizer, spraying the atomized solution on the filter paper material for 1min to wet the surface of the filter paper, taking out, washing with deionized water, washing with absolute ethyl alcohol, and drying at 80 ℃.
(3) And (3) treating the filter paper material obtained after drying in the step (2) in a cold plasma reaction chamber for 1min, wherein the plasma is discharged by dielectric barrier gas, the voltage is 75V, and the current is 0.3A.
(4) Adding a silver nitrate solution with the concentration of 10mmol/L into an ultrasonic atomizer, starting the ultrasonic atomizer to fully atomize the silver nitrate solution, applying a voltage of 15kV to a copper pipe to enable atomized fog drops to pass through the copper pipe, placing a filter paper material at a fog drop outlet below the copper pipe to enable the surface of the filter paper material to fully contact with the fog drops for 2min, taking out the filter paper material after treatment, washing with deionized water, and naturally drying.
The content and particle size distribution of silver particles supported on the cellulose paper in this example were substantially the same as in example 1.
Example 10
The calcium hydroxide solution in step (2) in example 9 was replaced with a 0.1mol/L sodium hydroxide solution, and the procedure was the same as in example 9.
The distribution and particle size of the nano-silver particles on the filter paper/nano-silver composite material prepared in this example are substantially the same as those in example 9.
The above-mentioned embodiments only express several embodiments of the present application, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the concept of the present application, which falls within the scope of protection of the present application. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (6)
1. A method for carrying nano silver particles on the surface of cellulose paper by in-situ reduction is characterized by comprising the following steps:
1) pretreating cellulose paper by using an alkaline solution;
2) treating the cellulose paper in cold plasma; the discharge mode of the cold plasma is dielectric barrier discharge, and the atmosphere is air or mixed gas of hydrogen and argon; in the cold plasma treatment process, the voltage is 50-100V, and the current is 0.2-0.5A;
3) the silver source solution is atomized by an ultrasonic atomizer, voltage is applied to atomized fog drops by a high-voltage direct-current power supply to enable the atomized fog drops to be inductively charged, the charged atomized fog drops are led to the surface of the cellulose paper, and nano silver particles are loaded on the surface of the cellulose paper in situ.
2. The method for in-situ reduction loading of nano-silver particles on the surface of cellulose paper according to claim 1, wherein the pretreatment mode comprises: the cellulose paper is soaked in an alkaline solution or sprayed on the surface of the cellulose paper by the alkaline solution.
3. The method for in-situ reduction of loaded nano-silver particles on the surface of cellulose paper as recited in claim 1, wherein the alkaline solution is sodium hydroxide solution or calcium hydroxide solution.
4. The method for in-situ reduction loading of nano-silver particles on the surface of cellulose paper according to claim 1, wherein the concentration of the alkaline solution is 0.05-0.2 mol/L.
5. The method for in-situ reduction of loaded nano-silver particles on the surface of cellulose paper as recited in claim 1, wherein the silver source solution is silver nitrate solution or silver ammonia solution.
6. The method for in-situ reduction loading of nano-silver particles on the surface of cellulose paper according to claim 1, wherein the voltage applied to the atomized droplets is 5-25 kV.
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| CN113201968B (en) * | 2021-05-10 | 2022-05-27 | 杭州众材科技股份有限公司 | Fading restoration method suitable for paper yellowing after deacidification |
| CN113430863B (en) * | 2021-07-21 | 2022-05-03 | 杭州众材科技股份有限公司 | Drying method for preventing paper from wrinkling and deforming after aqueous deacidification |
| CN114752958A (en) * | 2022-04-12 | 2022-07-15 | 西交利物浦大学 | Paper-based nano metal material and preparation method and application thereof |
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| CN109590028A (en) * | 2018-11-28 | 2019-04-09 | 浙江工商大学 | A method of nm-class catalyst is prepared using ultrasonic atomizatio plasma reaction |
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