CN109098040A - A kind of preparation method of supported nano zinc oxide function filter paper - Google Patents

A kind of preparation method of supported nano zinc oxide function filter paper Download PDF

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Publication number
CN109098040A
CN109098040A CN201810962089.8A CN201810962089A CN109098040A CN 109098040 A CN109098040 A CN 109098040A CN 201810962089 A CN201810962089 A CN 201810962089A CN 109098040 A CN109098040 A CN 109098040A
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filter paper
zinc oxide
nano zinc
supported nano
oxide function
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CN201810962089.8A
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CN109098040B (en
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鲁鹏
冯启明
吴敏
王志伟
高琳
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Guangxi University
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Guangxi University
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    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP 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
    • D21H27/00Special paper not otherwise provided for, e.g. made by multi-step processes
    • D21H27/08Filter paper
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP 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
    • D21H11/00Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D21H11/12Pulp from non-woody plants or crops, e.g. cotton, flax, straw, bagasse
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP 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
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20Macromolecular organic compounds
    • D21H17/33Synthetic macromolecular compounds
    • D21H17/34Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/35Polyalkenes, e.g. polystyrene
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP 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
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63Inorganic compounds
    • D21H17/64Alkaline compounds
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP 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
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63Inorganic compounds
    • D21H17/66Salts, e.g. alums
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP 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
    • D21H21/00Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/36Biocidal agents, e.g. fungicidal, bactericidal, insecticidal agents

Abstract

The invention discloses a kind of preparation methods of supported nano zinc oxide function filter paper, and this method comprises the following steps: 1) preparing the liquor zinci chloridi that mass concentration is 45%-65%;2) after liquor zinci chloridi being heated to 55 DEG C -85 DEG C, clean filter paper is totally submerged in liquor zinci chloridi, is taken out after impregnating 30s-2min, filter paper is washed with deionized, dries obtained filter paper substrate;3) material that total amount is reaction kettle volume 60-80% is added in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, wherein material is mixed by the filter paper substrate and aqueous slkali of step (2) by following consumption proportion: filter paper substrate 10-20g and aqueous slkali 50-100ml;Then 8-36h is reacted after reaction kettle being sealed at a temperature of 80-180 DEG C, is dried after filter paper is taken out and is washed with deionized after cooling to get supported nano zinc oxide function filter paper is arrived.Supported nano zinc oxide function filter paper of the invention has preferable photocatalysis antibacterial performance, and ZnO Nanocrystal can be made to be grown on the fiber of filter paper substrate, avoid secondary pollution, reusable, can be widely applied to water body purification and process field.

Description

A kind of preparation method of supported nano zinc oxide function filter paper
Technical field
The present invention relates to the preparation field of nano material, the preparation side of specifically a kind of supported nano zinc oxide function filter paper Method.
Background technique
Filter paper is made of criss-cross fiber, and this unique three-dimensional net structure makes filter paper have big surface area And porous structure, the good mechanical performance of filter paper and dimensional stability are assigned, can be used for being separated by filtration of solid/liquid, water The multiple fields such as body purification.In actual application, with the raising of the progress of nanotechnology and water process standard, in filter paper The some nano materials of fiber surface functionalization are opened, preparing, there is the filter paper of specific function to show bigger development prospect.It is common Filter paper fibre functionalization method be usually physical adherence method and chemical modification method, the nano material and paper of these methods modification are fine Bond strength between dimension is relatively weak, it is therefore necessary to find effective method for nanomaterial loadings in fiber surface.
Nano zine oxide not only has skin effect specific to nano material, amount as nanotechnology brand-new material Sub- dimensional effect etc., the advantages that being provided simultaneously with optics, the electricity, catalytic of zinc oxide, so that nano zine oxide is in many necks Domain suffers from critically important application value.By nano zine oxide in conjunction with cellulose fibre, supported nano zinc oxide function is prepared Filter paper, can assign the preferable anti-microbial property of paper and Photocatalytic Degradation Property, and expansion fiber element base filtering material is net in water body Change the application with water treatment field.
Currently, there are mainly two types of approach by the preparation process of supported nano zinc oxide function filter paper: (1) passing through conventional hydrothermal method Nano-ZnO is prepared, is then mixed by nano-ZnO with cellulose and nano-ZnO is compound on cellulosic substrates.However, nanometer Bond strength between ZnO and cellulose fibre is low so that the compound ability of nano-ZnO on cellulose is low, nano particle without Avoidable ground can enter in environment, cause secondary pollution, cause its application effect undesirable;(2) cellulosic substrates are impregnated In ZnO precursor solution, make Zn2+It interacts with cellulose, ZnO crystal is allowed to be nucleated growth directly on cellulosic substrates. The route is the problem is that operating procedure is complicated, and ZnO precursor is low with fibrin reaction accessibility, and nano-ZnO is in cellulose Upper compound quantity and combined strength bination are limited, and cellulose carrier is not involved in the control of ZnO nanocrystal size and shape.It is short in resource Scarce today, simplify supported nano zinc oxide function filter paper preparation process, realize conventional means be difficult to the fine structure obtained and Special performance, split green-emitting nano-functional material are of great significance.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of preparation methods of supported nano zinc oxide function filter paper, lead to The surface that ZnO Nanocrystal is grown in filter paper fibre is crossed, ZnO Nanocrystal is made to be firmly fixed to surface, Guarantee to assign filter paper excellent anti-microbial property while filter paper has preferable water filtering performance, while avoiding nano particle to disperse As treated, water body enters the ecosystem to the form of body together causes adverse effect.
The present invention solves above-mentioned technical problem with following technical solution:
A kind of preparation method of supported nano zinc oxide function filter paper of the present invention, including following operating procedure:
(1) prepare liquor zinci chloridi: in deionized water by zinc chloride powder dissolution, being configured to mass concentration is 45%- 65% liquor zinci chloridi;
(2) filter paper substrate is prepared: after liquor zinci chloridi made from step (1) is heated to 55 DEG C -85 DEG C, by clean filter paper It is totally submerged in liquor zinci chloridi, is taken out after impregnating 30s-2min, the filter paper of taking-up is washed with deionized until washing There is no Zn in liquid2+In the presence of dry in 50 DEG C of baking oven that filter paper substrate is made for 24 hours;
(3) it prepares supported nano zinc oxide function filter paper: the material that total amount is reaction kettle volume 60-80% being added to poly- In tetrafluoroethene hydrothermal reaction kettle, wherein material filter paper substrate as made from step (2) and aqueous slkali are mixed by following consumption proportion It closes: filter paper substrate 10-20g: aqueous slkali 50-100ml;Then 8- is reacted after reaction kettle being sealed at a temperature of 80-180 DEG C 36h, filter paper is taken out after cooling and be washed with deionized to pH value be 7,105 DEG C at a temperature of dry 12h receive to get to load Rice zinc oxide function filter paper.
Filter paper in the step (2) is quantitative 80-140g/m2Cotton fiber filter paper.
In the step (3), aqueous slkali includes sodium hydrate aqueous solution, ammonia aqueous solution, aqueous solution of urea.
In the step (3), the pH value of aqueous slkali is 9-12.
The method of the present invention has the following beneficial effects:
1, the method for the present invention can be such that ZnO Nanocrystal is grown directly upon on filter paper fibre, so that ZnO Nanocrystal It is firmly fixed to surface, to guarantee to assign filter paper excellent antibiotic property while filter paper has preferable water filtering performance Can, while avoiding nano particle water body enters the ecosystem together causes bad shadow as treated in the form of dispersion It rings.
2. preparation process of the present invention is simple, the raw material of use are easily obtained, and preparation process is economic and environment-friendly, secure nanometer Zincite crystal, convenient for recycling, meanwhile, it is reusable after functional paper cleaning, the utilization rate of nano zine oxide is improved, to expansion The industrial applications range of exhibition nano zine oxide functional paper is of great significance.
Figure of description
Fig. 1 is the scanning electron microscope (SEM) photograph of supported nano zinc oxide functional paper prepared by embodiment 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of supported nano zinc oxide functional paper prepared by embodiment 2.
Fig. 3 is the scanning electron microscope (SEM) photograph of supported nano zinc oxide functional paper prepared by embodiment 3.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention Content is not limited solely to the following examples.
Embodiment 1
A kind of preparation method of supported nano zinc oxide function filter paper, operating procedure are as follows:
(1) it prepares dipping liquor zinci chloridi: weighing the zinc chloride powder of 45g, be dissolved in the deionized water of 55g, add Hot and stirring is configured to the liquor zinci chloridi that concentration is 45% to being completely dissolved;
(2) filter paper substrate is prepared: after liquor zinci chloridi prepared by step (1) is heated to 55 DEG C, by quantitative 80g/m2's Cotton fiber filter paper is placed in liquor zinci chloridi, is totally submerged filter paper, is taken out after impregnating 30s, by the filter paper deionization of taking-up Water washing is until there is no Zn in cleaning solution2+In the presence of, in 50 DEG C of baking oven it is dry for 24 hours.
(3) it prepares supported nano zinc oxide function filter paper: the material that total amount is reaction kettle volume 60% is added to poly- four In vinyl fluoride hydrothermal reaction kettle, wherein the composition of material is according to the following ratio: filter paper substrate 10g:50ml pH made from step (2) The sodium hydrate aqueous solution that value is 10;8h is reacted after reaction kettle is sealed at a temperature of 80 DEG C, filter paper is taken out after cooling and is used in combination Deionized water wash to pH value be 7,105 DEG C at a temperature of dry 12h, obtain supported nano zinc oxide function filter paper;
Supported nano zinc oxide function filter paper is subjected to antibacterial experiment, it is to Escherichia coli and Listeria as the result is shown Bacteriostasis rate is 77.3%.Processing is filtered to infected water with supported nano zinc oxide function filter paper, water filtering performance is good, pure Water flux is 286.8Ls-1m-2, after reusing 20 times, still have good filter effect and fungistatic effect.
Embodiment 2
A kind of preparation method of supported nano zinc oxide function filter paper, operating procedure are as follows:
(1) it prepares dipping liquor zinci chloridi: weighing the zinc chloride powder of 55g, be dissolved in the deionized water of 45g, add Hot and stirring is configured to the liquor zinci chloridi that concentration is 55% to being completely dissolved;
(2) filter paper substrate is prepared: after liquor zinci chloridi prepared by step (1) is heated to 70 DEG C, by quantitative 110g/m2's Cotton fiber filter paper is placed in liquor zinci chloridi, is totally submerged filter paper, is taken out after impregnating 1min, by the filter paper deionization of taking-up Water washing is until there is no Zn in cleaning solution2+In the presence of, in 50 DEG C of baking oven it is dry for 24 hours.
(3) it prepares supported nano zinc oxide function filter paper: the material that total amount is reaction kettle volume 70% is added to poly- four In vinyl fluoride hydrothermal reaction kettle, wherein the composition of material is according to the following ratio: filter paper substrate 15g:75ml pH made from step (2) The aqueous solution of urea that value is 11;18h is reacted after reaction kettle is sealed at a temperature of 120 DEG C, filter paper is taken out and spent after cooling Ion water washing pH value dry 12h at a temperature of being 7,105 DEG C, obtains supported nano zinc oxide function filter paper;
Supported nano zinc oxide function filter paper is subjected to antibacterial experiment, it is to Escherichia coli and Listeria as the result is shown Bacteriostasis rate is 89.9%.Processing is filtered to infected water with supported nano zinc oxide function filter paper, water filtering performance is good, pure Water flux is 260.5Ls-1m-2, after reusing 20 times, still have good filter effect and fungistatic effect.
Embodiment 3
A kind of preparation method of supported nano zinc oxide function filter paper, operating procedure are as follows:
(1) it prepares dipping liquor zinci chloridi: weighing the zinc chloride powder of 65g, be dissolved in the deionized water of 35g, add Hot and stirring is configured to the liquor zinci chloridi that concentration is 65% to being completely dissolved;
(2) filter paper substrate is prepared: after liquor zinci chloridi prepared by step (1) is heated to 85 DEG C, by quantitative 140g/m2's Cotton fiber filter paper is placed in liquor zinci chloridi, is totally submerged filter paper, is taken out after impregnating 2min, by the filter paper deionization of taking-up Water washing is until there is no Zn in cleaning solution2+In the presence of, in 50 DEG C of baking oven it is dry for 24 hours.
(3) it prepares supported nano zinc oxide function filter paper: the material that total amount is reaction kettle volume 80% is added to poly- four In vinyl fluoride hydrothermal reaction kettle, wherein the composition of material is according to the following ratio: filter paper substrate 20g:100mlpH made from step (2) The ammonia aqueous solution that value is 12;36h is reacted after reaction kettle is sealed at a temperature of 180 DEG C, filter paper is taken out and spent after cooling Ion water washing pH value dry 12h at a temperature of being 7,105 DEG C, obtains supported nano zinc oxide function filter paper;
Supported nano zinc oxide function filter paper is subjected to antibacterial experiment, it is to Escherichia coli and Listeria as the result is shown Bacteriostasis rate is 95.7%.Processing is filtered to infected water with supported nano zinc oxide function filter paper, water filtering performance is good, pure Water flux is 306.5Ls-1m-2, after reusing 20 times, still have good filter effect and fungistatic effect.

Claims (4)

1. a kind of preparation method of supported nano zinc oxide function filter paper, which is characterized in that it includes following operating procedure:
(1) prepare liquor zinci chloridi: in deionized water by zinc chloride powder dissolution, being configured to mass concentration is 45%-65% Liquor zinci chloridi;
(2) filter paper substrate is prepared: after liquor zinci chloridi made from step (1) is heated to 55 DEG C -85 DEG C, clean filter paper is complete It is immersed in liquor zinci chloridi, is taken out after impregnating 30s-2min, the filter paper of taking-up is washed with deionized until in cleaning solution There is no Zn2+In the presence of dry in 50 DEG C of baking oven that filter paper substrate is made for 24 hours;
(3) it prepares supported nano zinc oxide function filter paper: the material that total amount is reaction kettle volume 60-80% is added to polytetrafluoro In ethylene hydrothermal reaction kettle, wherein material filter paper substrate as made from step (2) mixed with aqueous slkali by following consumption proportion and At: filter paper substrate 10-20g: aqueous slkali 50-100ml;Then 8-36h is reacted after reaction kettle being sealed at a temperature of 80-180 DEG C, Filter paper is taken out after cooling and be washed with deionized to pH value be 7,105 DEG C at a temperature of dry 12h to get to load nano oxygen Change zinc function filter paper.
2. the preparation method of supported nano zinc oxide function filter paper according to claim 1, it is characterised in that: the step (2) filter paper in is quantitative 80-140g/m2Cotton fiber filter paper.
3. the preparation method of supported nano zinc oxide function filter paper according to claim 1 or claim 2, it is characterised in that: step (3) In, the aqueous slkali includes sodium hydrate aqueous solution, ammonia aqueous solution, aqueous solution of urea.
4. the preparation method of supported nano zinc oxide function filter paper according to claim 1 or claim 2, it is characterised in that: step (3) In, the pH value of the aqueous slkali is 9-12.
CN201810962089.8A 2018-08-22 2018-08-22 Preparation method of functional filter paper loaded with nano zinc oxide Active CN109098040B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109440524A (en) * 2018-10-15 2019-03-08 广西大学 A kind of preparation method of supported nano zinc oxide anti-bacteria paper
CN114134705A (en) * 2021-11-23 2022-03-04 福建农林大学 Antibacterial and antiviral plant fiber prepared by using zinc chloride/urea eutectic system, and method and application thereof

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CN102898681A (en) * 2012-09-27 2013-01-30 河南科技大学 Loaded type nano-zinc oxide composite material
CN103194885A (en) * 2013-04-19 2013-07-10 中国民航大学 Method for microwave synthesis of nano-ZnO assembled cotton fibers
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CN106835673A (en) * 2017-03-27 2017-06-13 广西科技大学 A kind of UV resistance zinc oxide silk composite fiber and preparation method thereof
CN107237043A (en) * 2017-06-23 2017-10-10 苏州大学 Load the preparation method of the tunica fibrosa of oriented zinc oxide nanometer rods
CN108355636A (en) * 2018-03-20 2018-08-03 商丘师范学院 A kind of high efficiency preparation method of carbon doped zinc oxide nano composite material

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CN102691204A (en) * 2012-05-30 2012-09-26 南通大学 Preparation method of nano-zinc-oxide-loaded antibacterial ultraviolet-resistant fibers or textiles
CN102898681A (en) * 2012-09-27 2013-01-30 河南科技大学 Loaded type nano-zinc oxide composite material
CN103194885A (en) * 2013-04-19 2013-07-10 中国民航大学 Method for microwave synthesis of nano-ZnO assembled cotton fibers
CN105854949A (en) * 2015-01-23 2016-08-17 中国科学院宁波材料技术与工程研究所 Cellulose/nano zinc oxide composite material and preparation method and application thereof
CN105442298A (en) * 2015-12-17 2016-03-30 浙江理工大学 Preparation method for ultrasound-assisted fiber surface expanding of nonwoven cloth and loading with nano zinc oxide
CN106243786A (en) * 2016-07-29 2016-12-21 贵州大学 A kind of preparation method of the fabric ultraviolet resistant of simple and efficient
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CN107237043A (en) * 2017-06-23 2017-10-10 苏州大学 Load the preparation method of the tunica fibrosa of oriented zinc oxide nanometer rods
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CN114134705A (en) * 2021-11-23 2022-03-04 福建农林大学 Antibacterial and antiviral plant fiber prepared by using zinc chloride/urea eutectic system, and method and application thereof

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