CN104524866A - Composite antibacterial air filtration material and preparation method thereof - Google Patents
Composite antibacterial air filtration material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of an air filtration material, especially to a composite antibacterial air filtration material and its preparation method. The composite antibacterial air filtration material contains at least a layer of a non-woven base-material, network-structured cellulose nanofiber formed between fibers of the non-woven base-material and chitosan loaded on the surface of fibers of the non-woven base-material and/or the cellulose nanofiber. By introducing cellulose nanofiber and chitosan into the inside of common non-woven fabric, the network structure of cellulose nanofiber is formed between fibers of the non-woven fiber. Pore diameter of the non-woven fabric is reduced, specific surface area of the non-woven fabric is increased, and service life of the non-woven fabric is prolonged. By further utilization of antibacterial performance of chitosan, the high-efficiency low-resistance composite air filtration material with antibacterial performance is obtained.
Description
Technical field
The present invention relates to air filting material technical field, particularly a kind of composite antibacterial air filting material, and preparation method thereof.
Background technology
Current, the situation is tense in In The Atmosphere Over China pollution.According to the urban air-quality daily paper that Chinese Ministry of Environmental Protection announces January in this year, front 10 cities that API (Air Pollution Index) pollution index is the highest are: Shijiazhuang, Handan, Baoding, Tangshan, Tianjin, Zhengzhou, Jinan, Qinhuangdao, Jining, Urumchi and Wuhan (side by side).It is the most harmful for having the air pollution of two kinds of forms to be confirmed as the mankind by ALA (ALA), and it comprises: (1) gas pollutant, as ozone, mist, VOC (VOC) etc.; (2) Particulate Pollution, as cigarette and dust.
Above-mentioned rank does not also comprise PM2.5 and ozone pollution index.Particulate pollutant occupies a tiny space in all kinds of pollution, and the healthy of people in its serious harm.Its important sources is the particle that the fuel combustions such as the coal burnings such as power plant, vehicle and jumbo produce.In addition the burning of timber, stalk also can produce Particulate Pollution.
Wherein the ground air quality such as Beijing, Hebei, Shandong reaches severe contamination, PM2.5 index presses on towards maximum, as Shijiazhuang, Handan, Xingtai, Hengshui air quality index even " quick-fried table ", numerical value has met or exceeded the measurement upper limit of 500, primary pollutant mostly is PM2.5, PM10, Pekinese PM2.5 value breakthrough 900.
Air pollution can not only pass through physics, chemistry, biological corrosion function, produces damaging influence to surrounding objects; And dusty gas also through positions such as respiratory system (lung), epiderm skins, can produce toxic action to respiratory system, nervous system, immunocompetence, skin, liver, internal system etc.And the state of mind of people can be affected, easily there is the bad reaction such as fatigue, anxiety, reduce work, learning efficiency.Live and work in the long-term environment poor in air quality, not only can cause that respiratory function declines, respiratory symptom increases the weight of, also can cause the diseases such as chronic bronchitis, bronchial astehma, pulmonary emphysema, the serious increase that also can cause lung cancer, nasopharyngeal carcinoma illness rate.Therefore, become increasingly conspicuous with the regional atmospheric environment problem that pellet (PM10), fine particle (PM2.5) are characteristic contamination, infringement body health of people, affect social harmony and stablize, In The Atmosphere Over China pollution control is very urgent.
For ensureing the clean of personal health and working environment, air filting material is widely used in the every field such as semicon industry, pharmacy and food service industry, auto industry, nuclear industry, building trade.Along with the development of science and technology and the enhancing of people's consciousness of self-protection, market is also increasing to the demand of filtering material.
The performance indications evaluating air filting material quality mainly contain efficiency, resistance, dust containing capacity and flux four aspects.The performance of type to air filting material of fiber-like filtering material plays decisive role.The combined composite fibre air filting material of ball line that CN103706182A adopts electrostatic spinning to prepare.Leung finds, at the laminated micrometer fibers felt in nanofiber mats surface, can increase filter efficiency, and pressure drop to be less than pure nanofiber mats.The first electrospinning such as Wang goes out polyacrylonitrile (PAN) fibrage, then forms composite filter material above being covered by polyvinyl alcohol (PVA) nanofiber.
Above-mentioned research is all adopt the way of electrostatic spinning to improve filter efficiency, but pressure drop increases also thereupon, is difficult to the effect reaching high efficiency, low pressure drop.And the industrialization of electrostatic spinning is difficult, be difficult to the product of formation scale.Even if there is product out, cost is also higher.How prepared the filtering material of efficient low-resistance by simple mode, become one of focus paid close attention in air filting material field.
Summary of the invention
The present invention aims to provide that a kind of filter efficiency is high, and Pressure Drop is little, and has the composite air filtering material of anti-microbial property.
For achieving the above object, the present invention is by the following technical solutions:
On the one hand, a kind of composite antibacterial air filting material is provided, comprise: at least one deck non-woven fabrics base material, formed between the fiber sticking in described non-woven fabrics base material cellulose nano-fibrous (CNF) of network structure, and the fiber of load at non-woven fabrics base material and/or the shitosan (CS) on described cellulose nano-fibrous surface.
In some embodiments, described cellulose nano-fibrous surface can have electronegative carboxylic group.
In some embodiments, described cellulose nano-fibrous length can be 0.5-5 μm, width can be 4-10nm, and draw ratio can be 50-1250.
In some embodiments, the weight of described non-woven fabrics base material can be 15-100g/m
2.
In some embodiments, described non-woven fabrics base material is selected from: spun-bonded non-woven fabrics, melt spraying non-woven fabrics, needle punched non-woven fabrics, spunlace non-woven cloth, bamboo-carbon fibre non-woven fabrics, anion nanometer non-woven fabrics, nano-silver ionic non-woven fabrics, or their any combination.
On the other hand, a kind of method preparing claim described composite antibacterial air filting material of the present invention is provided, comprise: comprise cellulose nano-fibrous and solution that is shitosan by flooding and/or spraying, described in cellulose nano-fibrous and shitosan is attached at least in one deck non-woven fabrics base material, and dry.
In some embodiments, the step of described dipping and/or spraying comprises: be immersed in by described at least one deck non-woven fabrics base material and comprise in the solution of shitosan, and after taking-up, spraying comprises cellulose nano-fibrous solution.
In some embodiments, the step of described dipping and/or spraying comprises: in different non-woven fabrics base materials, floods respectively and/or sprays the solution comprising cellulose nano-fibrous solution He comprise shitosan; Laminating comprises cellulose nano-fibrous and described non-woven fabrics base material that is shitosan respectively, makes chitosan penetrating to comprising cellulose nano-fibrous nonwoven fabric base sheet material layers and in interface plastic; Comprise the non-woven fabrics base material of shitosan described in removal, obtain comprising shitosan and both non-woven fabrics base material cellulose nano-fibrous.
In some embodiments, described in comprise in cellulose nano-fibrous solution and can also comprise surfactant.
Beneficial effect of the present invention is: cellulose nano-fibrous and shitosan are introduced common non-woven fabrics inner, make cellulose nano-fibrously between non-woven fabrics fiber, to form network structure, reduce the aperture of non-woven fabrics, increase the specific area of non-woven fabrics, extend the service life of non-woven fabrics; Utilize the anti-microbial property of shitosan further, obtain the efficient low-resistance composite air filtering material with anti-microbial property.
Accompanying drawing explanation
Fig. 1 is that the CNF/ shitosan/PET compound nonwoven cloth SEM according to embodiment 1 schemes.
Fig. 2 is that the CNF/ shitosan/PP compound nonwoven cloth SEM according to embodiment 2 schemes.
Detailed description of the invention
Cellulose nano-fibrous diameter, usually in the scope of several nanometer, because of minimum size, makes it have great specific area; And its chemical stability, mechanical property, heat endurance and eco-friendly performance, make this material can be applied to the fields such as nano-complex, nanometer paper and organizational project.
Chitosan-phospholipid complex has good antibacterial activity, can suppress the growth and breeding of some fungies, bacterium and virus.Think that by the end of 2013 its possible mechanism has be polycation due to shitosan at three: one, easily electronegative with fungal cell surface group effect, thus the mobility of change pathogen cell membrane and permeability; Two is copying and transcribing of interference DNA; Three is block pathogen metabolism.
Since 2010, have many researchers to propose shitosan by induction pathogenesis-related proteins, mode such as accumulation secondary metabolite and intracellular signaling etc. reaches the viewpoint of antibacterial object.Papineau etc. think, due to the interaction of negative electrical charge on the positive charge of chitosan molecule and bacterial cell membrane, intracellular protease and other compositions are leaked, thus reach antibacterial, bactericidal action.Sudharshan etc. point out, due to shitosan can to infiltrate in the core of bacterium and and DNA combine, the synthesis of suppression mRNA, thus hinder the synthesis of mRNA and protein, reaches antibacterial action.
The present inventor is by cellulose nano-fibrous and shitosan, introduce common non-woven fabrics (it is as fiber filter media) inner, cellulose nano-fibrous sticking between non-woven fabrics fiber is made to form network structure, reduce the aperture of non-woven fabrics, increase the specific area of non-woven fabrics, extend the service life of non-woven fabrics.Use cellulose nano-fibrous with negative electrical charge of surface, it can have stronger interaction with positively charged shitosan, further shitosan is also introduced non-woven fabrics inside, and combines closely simultaneously; Reach the object reducing fiber filter media aperture, make it have anti-microbial property, obtain the composite efficient low-resistance air filting material with anti-microbial property.
Visible, composite antibacterial air filting material of the present invention mainly comprises three parts, non-woven fabrics base material, and it can comprise one or more layers; Cellulose nano-fibrous, it sticks between the fiber of non-woven fabrics base material, and forms network structure; And shitosan, its load is on the fiber of non-woven fabrics base material and/or cellulose nano-fibrous surface.
Non-woven fabrics base material can comprise spun-bonded non-woven fabrics layer, melt-blown nonwoven layer of cloth, acupuncture nonwoven layer of cloth, spunlace non-woven cloth layer, bamboo-carbon fibre nonwoven layer, anion nanometer nonwoven layer, nano-silver ionic nonwoven layer, etc.Non-woven fabrics base material can have one deck or multilayer bonded to each other, and when there being multi-layer nonwoven fabrics base material, each layer can be identical or different.Based on object of the present invention, the weight of non-woven fabrics base material can be 15-100g/m
2.
Cellulose nano-fibrous and shitosan can comprise cellulose nano-fibrous and solution (especially aqueous dispersion liquid) that is shitosan by solution impregnation and/or spraying, and is loaded on non-woven fabrics base material.Thus cellulose nano-fibrous and shitosan can be co-located on (such as can be uniformly distributed) on whole non-woven fabrics base material.The cellulose nano-fibrous major diameter prepared traditionally is smaller, disperse not.Based on object of the present invention in some cases, can use and there is the cellulose nano-fibrous of following characteristic: its length can be 0.5-5 μm, width can be 4-10nm, and draw ratio can be 50-1250.Further, in order to give air filting material endowing antibacterial energy of the present invention, preferably using surface to have the cellulose nano-fibrous of electronegative carboxylic group, thus there is the ability of viral adsorption and heavy metal ion.And the cellulose nano-fibrous further modification that exists for of carboxylic group provides functional group.
Like this cellulose nano-fibrous such as can be prepared as follows: adopt N-oxo-compound/bromide or iodide/oxidizer system, to prepare cellulose nano-fibrous aqueous dispersion liquid.This preparation process is simple, and the cellulose nano-fibrous diameter obtained is evenly distributed.
It should be noted that, the preparation of cellulose nano-fibrous aqueous dispersion liquid is not limited only to methods described herein, and the method stated herein just prepares the one in all multi-methods of cellulose nano-fibrous aqueous dispersion liquid.
Particularly, the aqueous liquid dispersion that following preparation is cellulose nano-fibrous.
First, oxycellulose.Cellulose is added in the water being dissolved with N-oxo-compound and bromide or iodide, makes suspension; In oxidizer system solution, drip aqueous slkali again and be adjusted to alkalescence, such as pH=10; Start reaction by adding oxidizing agent solution, reaction temperature is normal temperature, maintains alkaline environment (such as maintaining pH is 10) in course of reaction by adding aqueous slkali.When aqueous slkali does not need to consume, reaction can terminate, and adds ethanol and stops reaction.Add water, filter, thoroughly to clean the cellulose through oxidation.
Then, mechanical treatment.Stir the suspension of cellulose in water through oxidation, agitator speed is 1500rpm-15000rpm, and mixing time is 6 little of 10 days, obtains solution or the suspension of different transparency.Substantially, the carboxyl-content on cellulose is more, mixing time is longer, mixing speed is faster, is more conducive to the solution obtaining transparent clarification.
Be applicable to cellulose of the present invention and for being derived from the wood pulp of various trees, or the non-woody pulp of cotton, fiber crops, bamboo and straw etc. can be derived from; Form can be the paper pulp of drying, or the magma of undried.
N-oxo-compound can select 2,2,6,6-tetramethyl piperidine-1-oxide radical (TEMPO), 2,2,6,6-tetramethyl piperidine-N-oxygen bases, 2,2,6,6-tetramethyl-4-acryloyl-oxy phenylpiperidines-1-oxygen bases etc.Bromide or iodide can be the alkali metal salts such as sodium bromide or KI.Oxidant can be the hypohalogenous acids of the halogens such as chlorine, bromine and iodine, halous acid or high hydracid and their salt.Regulating oxidizer system solution to be alkalescence acid used can be hydrochloric acid, sulfuric acid, oxalic acid, citric acid or acetic acid, etc.The alkali maintaining alkaline environment used can be NaOH, potassium hydroxide, lithium hydroxide or organic base, etc.
In the cellulose nano-fibrous aqueous dispersion liquid so obtained, cellulose nano-fibrous length is 0.5-5 μm, and width only has 4-10nm, and draw ratio is 50-1250.The solid content of aqueous dispersion liquid can be 0.01-0.7%, carboxyl-content can be 0.2-3.6mmol/g, if carboxyl amount is lower than 0.2mmol/g, then be difficult to obtain the cellulose nano-fibrous of above-mentioned diameter, if higher than 3.6mmol/g, then degree of crystallinity significantly reduces, and under making high humidity environment, barrier properties for gases is deteriorated.The pH value of aqueous dispersion liquid can be 3-8.
Shitosan can adopt commercially available Chitosan-phospholipid complex, comprising: using carboxyl chitosan (mostly should being used as is CMC); Shitosan salt (common are chitosan hydrochloride, chitosan quaternary ammonium salt, chitosan lactate, glutamate etc.); Sulfated chitosan; Chitosan oligosaccharide; Hyaluronic acid-like chitosan, etc.During preparation, shitosan is dissolved in obtained chitosan solution in dilute acetic acid solutions.
Two kinds of modes can be had to carry out flooding and/or spraying.Non-woven fabrics base material formerly impregnated in chitosan solution by the first, after taking-up, more cellulose nano-fibrous aqueous dispersion liquid is sprayed on the non-woven fabrics base material surface being soaked with chitosan solution; Another kind of mode is first in different non-woven fabrics base materials, floods respectively and/or sprays the solution comprising cellulose nano-fibrous solution He comprise shitosan, and the nonwoven fabric base sheet material layers of then fitting different.Chitosan solution constantly permeates downwards, and in non-woven fabrics near interface plastic.This step such as can be achieved on upper strata by making the non-woven fabrics base material being soaked with chitosan solution.Remove upper strata non-woven fabrics after a period of time, after drying lower nonwoven cloth, form more uniform network structure.
For making solution can infiltrate preferably in comparatively hydrophobic non-woven fabrics base material, surfactant can be added comprising in cellulose nano-fibrous solution, such as, ionic and/or the nonionic surface active agent of inertia can be selected.
It is inner that common non-woven fabrics introduced by cellulose nano-fibrous and shitosan by the present invention, makes cellulose nano-fibrously between non-woven fabrics fiber, to form network structure, reduces the aperture of non-woven fabrics, increase the specific area of non-woven fabrics, extend the service life of non-woven fabrics; Further introducing shitosan, utilizes its anti-microbial property, obtains the efficient low-resistance composite air filtering material with anti-microbial property.
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and the specific embodiments, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, and be not construed as limiting the invention.
Embodiment 1
Adopt 2,2,6,6-tetramethyl piperidine-1-oxide radical TEMPO/ sodium bromide (NaBr)/clorox (NaClO) system, lignocellulosic is oxidized, subsequently mechanical treatment, prepares cellulose nano-fibrous aqueous dispersion liquid.
Particularly, 30g cellulose is joined in the 4L water containing 4gNaBr and 0.48gTEMPO, make suspension; In NaClO solution, drip HCl regulate pH=10, then NaClO is joined in solution according to the cellulosic concentration of 6.0mmol/g, start reaction, reaction normal temperature carries out, and is 10, when no longer consuming NaOH by adding NaOH solution maintenance pH, namely reaction terminates, and adds 50g ethanol, cessation reaction.
Washing, filter through oxidation cellulose, by through oxidation the suspension of cellulose in water stir 10 days in the agitator of rotating speed 1500rpm, obtain comparatively transparent cellulose nano-fibrous aqueous dispersion liquid.Cellulose nano-fibrous length is 0.5-5 μm, width can be 4-10nm, and draw ratio can be 50-1250.
Regulate the solid content of cellulose nano-fibrous aqueous dispersion liquid to be 0.3%, drip HCl and regulate pH=6, trying to achieve carboxyl-content by the NaOH solution of 0.1mol/l by electrical conductivity titration is 1mmol/g, and the last pH value of dispersion liquid is arranged on 6.The final concentration adjustment of CNF dispersion liquid is 0.05% for subsequent use.
Shitosan is dissolved in the chitosan solution of in the acetic acid solution of 1 (v/v) % obtained 0.05%, records PH and be about 4.
By 100g/m
2pETG (PET) needle punched non-woven fabrics impregnated in after the chitosan solution of 0.05% and take out tiling on a glass, the CNF dispersion liquid of 0.05% is sprayed on the PET needle punched non-woven fabrics surface being soaked with chitosan solution, for improving the wellability of CNF dispersion liquid in PET needle punched non-woven fabrics, add 0.001% DOW CORNING DC-193 surfactant.By CNF/CS/PET compound nonwoven cloth 80 DEG C oven dry.
The SEM figure of the CNF/CS/PET compound nonwoven cloth obtained as shown in Figure 1.CNF and CS sticks on the fiber of non-woven fabrics, forms network structure.
Embodiment 2
Adopt 2,2,6,6-tetramethyl-4-acryloyl-oxy phenylpiperidines-1-oxygen base/sodium iodide (NaI)/sodium hypobromite (NaBrO) system, cotton fibre element is oxidized, subsequently mechanical treatment, prepares cellulose nano-fibrous aqueous dispersion liquid.
20g cellulose is joined containing 7gNaI and 0.6g2, in the 3L water of 2,6,6-tetramethyl piperidine-N-oxygen base, makes suspension; H is dripped in NaBrO solution
2sO
4regulate pH=10, then join in solution by NaBrO according to the cellulosic concentration of 6.5mmol/g, start reaction, reaction normal temperature carries out, and maintaining pH by interpolation KOH solution is 10, and when no longer consuming NaOH, namely reaction terminates, and adds 60g ethanol, cessation reaction.
Washing, filter cellulose through oxidation, be stir 6 hours in the agitator of 15000rpm in rotating speed by the suspension of cellulose in water through oxidation, obtain comparatively transparent cellulose nano-fibrous aqueous dispersion liquid.Cellulose nano-fibrous length is 0.5-5 μm, width can be 4-10nm, and draw ratio can be 50-1250.。
Regulate the solid content of cellulose nano-fibrous aqueous dispersion liquid to be 0.4%, drip HCl and regulate pH=6, trying to achieve carboxyl-content by the NaOH solution of 0.05mol/l by electrical conductivity titration is 2mmol/g, and the last pH value of dispersion liquid is arranged on 7.5.The final concentration adjustment of CNF dispersion liquid is 0.02% for subsequent use.DOW CORNING DC 29 surfactant of 0.003% is added in the CNF dispersion liquid of 0.02%.
Chitosan oligosaccharide is dissolved in the chitosan solution of in deionized water obtained 0.02%, in the chitosan solution of 0.02%, adds DOW CORNING DC 29 surfactant of 0.003%.
By 35g/m
2polypropylene (PP) melt spraying non-woven fabrics immerse in CNF solution, PP melt spraying non-woven fabrics onesize for another block is immersed in chitosan solution, then the two is gathered into folds, be soaked with the PP melt spraying non-woven fabrics of shitosan upper, chitosan solution constantly permeates downwards, and near interface plastic, keep 5 minutes, taken off by upper strata PP melt spraying non-woven fabrics, dry lower floor PP melt spraying non-woven fabrics for 60 DEG C, CNF and shitosan form more uniform network structure in base material non-woven fabrics.
The SEM figure of the CNF/CS/PP compound nonwoven cloth obtained as shown in Figure 2.CNF and CS sticks on the fiber of non-woven fabrics, forms network structure.
Adopt TSI8130 filtrate tester, the strainability of the composite antibacterial air filting material of testing example 1 and 2, and use reference examples 1 (PET needle punched non-woven fabrics) and reference examples 2 (PP melt spraying non-woven fabrics) in contrast.Aerosol adopts quantity median particle diameter to be the NaCl of 75nm, and detecting flow is (85 ± 4) l/min, and test result is as shown in table 1.
The strainability of table 1 composite antibacterial air filting material
From the data of table 1, composite antibacterial air filting material filter efficiency of the present invention is up to more than 99.8%, and Pressure Drop is then only a little more than independent non-woven fabrics.
The above the specific embodiment of the present invention, does not form limiting the scope of the present invention.Any various other done by technical conceive of the present invention change and distortion accordingly, all should be included in the protection domain of the claims in the present invention.
Claims (9)
1. a composite antibacterial air filting material, is characterized in that, comprising:
At least one deck non-woven fabrics base material, forms the cellulose nano-fibrous of network structure between the fiber sticking in described non-woven fabrics base material, and the fiber of load at non-woven fabrics base material and/or the shitosan on described cellulose nano-fibrous surface.
2. composite antibacterial air filting material as claimed in claim 1, it is characterized in that, described cellulose nano-fibrous surface has electronegative carboxylic group.
3. composite antibacterial air filting material as claimed in claim 1, it is characterized in that, described cellulose nano-fibrous length is 0.5-5 μm, width is 4-10nm, and draw ratio is 50-1250.
4. composite antibacterial air filting material as claimed in claim 1, it is characterized in that, the weight of described non-woven fabrics base material is 15-100g/m
2.
5. composite antibacterial air filting material as claimed in claim 1, it is characterized in that, described non-woven fabrics base material is selected from: spun-bonded non-woven fabrics, melt spraying non-woven fabrics, needle punched non-woven fabrics, spunlace non-woven cloth, bamboo-carbon fibre non-woven fabrics, anion nanometer non-woven fabrics, nano-silver ionic non-woven fabrics, or their any combination.
6. prepare the method for the composite antibacterial air filting material described in claim 1-5 for one kind, it is characterized in that, comprise: comprise cellulose nano-fibrous and solution that is shitosan by flooding and/or spraying, make cellulose nano-fibrous and shitosan be attached to described at least in one deck non-woven fabrics base material, and to dry.
7. method as claimed in claim 6, it is characterized in that, the step of described dipping and/or spraying comprises:
Described at least one deck non-woven fabrics base material is immersed in and comprises in the solution of shitosan, and after taking-up, spraying comprises cellulose nano-fibrous solution.
8. method as claimed in claim 6, it is characterized in that, the step of described dipping and/or spraying comprises:
In different non-woven fabrics base materials, flood respectively and/or spray the solution comprising cellulose nano-fibrous solution He comprise shitosan;
Laminating comprises cellulose nano-fibrous and described non-woven fabrics base material that is shitosan respectively, makes chitosan penetrating to comprising cellulose nano-fibrous nonwoven fabric base sheet material layers and in interface plastic;
Comprise the non-woven fabrics base material of shitosan described in removal, obtain comprising shitosan and both non-woven fabrics base material cellulose nano-fibrous.
9. method according to any one of claim 6-8, is characterized in that, described in comprise in cellulose nano-fibrous solution and also comprise surfactant.
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| CN113731197B (en) * | 2021-09-17 | 2022-05-20 | 山东省科学院新材料研究所 | Preparation method of high-permeability antibacterial polyimide/chitosan composite nanofiber air filtering membrane, product and application thereof |
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