CN108118558A - A kind of silver-colored zinc zeolite antibacterial paper washer for loading plants essential oil and preparation method thereof - Google Patents
A kind of silver-colored zinc zeolite antibacterial paper washer for loading plants essential oil and preparation method thereof Download PDFInfo
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- CN108118558A CN108118558A CN201711344799.6A CN201711344799A CN108118558A CN 108118558 A CN108118558 A CN 108118558A CN 201711344799 A CN201711344799 A CN 201711344799A CN 108118558 A CN108118558 A CN 108118558A
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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
- D21H21/00—Non-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
- D21H21/14—Non-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
- D21H21/36—Biocidal agents, e.g. fungicidal, bactericidal, insecticidal agents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
- C01B33/28—Base exchange silicates, e.g. zeolites
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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
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/14—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
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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
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/14—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
- D21H19/34—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12 comprising cellulose or derivatives thereof
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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
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
- D21H27/002—Tissue paper; Absorbent paper
- D21H27/004—Tissue paper; Absorbent paper characterised by specific parameters
- D21H27/005—Tissue paper; Absorbent paper characterised by specific parameters relating to physical or mechanical properties, e.g. tensile strength, stretch, softness
- D21H27/007—Tissue paper; Absorbent paper characterised by specific parameters relating to physical or mechanical properties, e.g. tensile strength, stretch, softness relating to absorbency, e.g. amount or rate of water absorption, optionally in combination with other parameters relating to physical or mechanical properties
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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
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
- D21H27/10—Packing paper
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Abstract
A kind of silver-colored zinc zeolite antibacterial paper washer for loading plants essential oil, is prepared as follows obtaining：Added in after zeolite materials are dried in silver-colored zinc mixed solution, be dispersed with stirring and be placed at 40~60 DEG C 8~12h of heat preservation, after through filtering, washing, filtration cakes torrefaction, obtain silver-colored zinc zeolite；Gained silver-colored zinc zeolite is mixed with plants essential oil, sealing is placed on 2~4h of heat preservation at 80~100 DEG C, is cooled to room temperature, is washed with ether afterwards, obtains carrying oily silver-colored zinc zeolite；Gained is carried in oily silver-colored zinc zeolite, ethyl cellulose addition absolute ethyl alcohol, is dispersed with stirring at room temperature uniformly, obtains coating liquid, gained coating liquid is spread evenly across blotting paper surface, be protected from light natural drying at room temperature to get finished product；The present invention carries that oily silver-colored zinc zeolite antibacterial paper washer wide sterilization spectrum, stability is good and bacteriostasis, preservation excellent effect.
Description
(1) technical field
The invention belongs to packaging material for food fields, are related to a kind of antibacterial paper washer, and in particular to a kind of load plants essential oil
Silver-colored zinc zeolite antibacterial paper washer and preparation method thereof.
(2) technical background
Zeolite is the hydrous alumino silicates mineral of family's rack-like construction, and natural zeolite is evident in Jinyun county, Zhejiang province county of China, Liaoning
The ground such as Wu Xian, which have, largely to be contained, in addition by also being capable of a large amount of synthetic zeolites the methods of high temperature hydro-thermal method.Containing rich inside zeolite
Rich opening structure, and ion exchange can be carried out, thus it is widely used in sewage disposal.Japanese researchers' profit in 1984
Zeolite with carrying silver is prepared for the first time with the ion exchange property of zeolite, and finds zeolite with carrying silver to Escherichia coli, mould, withered grass bar
The microorganisms such as bacterium have good inhibition, are resistant to 200 DEG C of high temperature and performance is not decreased obviously.Afterwards in order to drop
The dosage of low silver ion and raising discoloration-resistant performance, and copper system, zinc system and more metal system antibacterial zeolite particles are gradually developed, at present
Most studied antibacterial zeolite particles or zeolite with carrying silver and silver-colored zinc bimetallic zeolite.
Ag+、Zn2+The antibacterial mechanisms of metal ions are waited, there are two types of explain for mainstream：1. haptoreaction hypothesis and 2. catalytic reaction
Hypothesis, it is considered that wherein based on the first sterilization mechanism, and catalytically bactericidal process also functions to certain effect.Newest research shows
Metal ion in antibacterial zeolite particles is unevenly distributed in entire zeolitic frameworks.Between metal ion and zeolite screen work atom
There are electrostatic attraction effects, enabling the metal ion of separate out is limited, thus the fungistatic effect of antibacterial zeolite particles is wrapped
The restriction of contact area between dress and food.Such as the fruits and vegetables shelf life such as red bayberry, edible mushroom is short, easy mildew corruption, and table
There are a large amount of holes, folds, the at this time antibacterial anti-corrosion effect of antibacterial zeolite particles packaging material in face to be just subject to above-mentioned reason and give a discount greatly
Button.Domestic《Inorganic silver-impregnated zeolite antibiotic papers and preparation method thereof》(101182689 B of CN) and《A kind of antibiosis layered board
And preparation method thereof》Patents of invention such as (CN 100411867C) are without the solution for being related to the problem.Correlation both domestic and external
In research preferable solution is also not yet proposed on this problem.
(3) content of the invention
The present invention is intended to provide a kind of wide sterilization spectrum, stability is good and the load oil silver-colored zinc zeolite of bacteriostasis, preservation excellent effect
Antibacterial paper washer and preparation method thereof.
Technical scheme is as follows：
A kind of silver-colored zinc zeolite antibacterial paper washer for loading plants essential oil, is prepared as follows obtaining：
(1) silver-colored zinc zeolite is prepared
Zeolite materials are placed at 80~100 DEG C dry 4~6h, according to solid-to-liquid ratio 1 after being cooled to room temperature：10~12 (w/
V, g/mL) add in silver-colored zinc mixed solution, be dispersed with stirring and be placed at 40~60 DEG C 8~12h of heat preservation, after through filtering, washing,
Filtration cakes torrefaction obtains silver-colored zinc zeolite；
The preparation method of the silver-colored zinc mixed solution is：By 0.1mol/L silver nitrate solutions and 0.5mol/L zinc nitrate solutions
By volume 1：0.25~4 (particularly preferred 1：0.25) mix to get；
The suction filtration preferably carries out decompression suction filtration with Medium speed filter paper；
The washing is preferably rinsed with pure water, and is rinsed to the silver ion in filtrate with 0.1mol/L sodium chloride
Until solution is examined without apparent white precipitate；
The concrete operations of the drying are：It will be placed in 60~80 DEG C of convection oven dry 10 by the filter cake of washing~
Then 12h is placed in 60~80 DEG C of vacuum drying oven dry 2~3h again, finally take out and be kept in dark place in shady place sealing；
(2) prepare and carry oily silver-colored zinc zeolite
Silver-colored zinc zeolite obtained by step (1) is mixed with plants essential oil, sealing is placed on 2~4h of heat preservation at 80~100 DEG C, it
Postcooling is washed with ether to room temperature, obtains carrying oily silver-colored zinc zeolite；
The volumetric usage of the plants essential oil is calculated as 0.5~0.75mL/g with the quality of silver-colored zinc zeolite；
The plants essential oil is cinnamic acid, carvacrol or Herba Origani Vulgaris quintessence oil；
Gained carries oily silver-colored zinc zeolite sealing and is kept in dark place；
(3) the silver-colored zinc zeolite antibacterial paper washer of load plants essential oil is prepared
Oily silver-colored zinc zeolite will be carried obtained by ethyl cellulose, step (2) to add in absolute ethyl alcohol, is dispersed with stirring at room temperature
It is even, coating liquid is obtained, gained coating liquid is spread evenly across blotting paper surface, is protected from light natural drying at room temperature to get described negative
Carry the silver-colored zinc zeolite antibacterial paper washer of plants essential oil；
The oily silver-colored zinc zeolite and the mass ratio of ethyl cellulose of carrying is 1：10~20；
The volumetric usage of the absolute ethyl alcohol is calculated as 50~200mL/g to carry the quality of oily silver-colored zinc zeolite；
The coating liquid can be used this field routine techniques and be coated on blotting paper surface, such as using Meyer stick by coating liquid
Blotting paper surface is evenly applied to, volatilization naturally is dried, and recommendation coating weight is 0.05~0.06mL/cm2。
Heretofore described room temperature is 20~30 DEG C.
Compared with common metal system zeolite antibacterial paper washer packaging, the present invention has the following advantages：
1. solving bacteriostasis property caused by metal system zeolite antimicrobial packaging paper washer is restricted by contact area to decline, significantly carry
The high effect of anti-bacterial refreshing.
The stability of conventional silver-colored zinc zeolite antimicrobial packaging paper washer is excellent, but silver, zinc ion are also by zeolite lattice hole
Powerful electrostatic force and dispersion force firmly fetter wherein, are often facing the contact area between packaging and food by limited time, are pressing down
Bacterium antiseptic property is unsatisfactory.Such as Fig. 6 A, the anti-corrosion effect of antibacterial pad is to having a competition made of silver-colored zinc zeolite and the oily silver-colored zinc zeolite of load
It tests as can be seen that conventional silver-colored zinc zeolite antibacterial paper washer can not prevent red bayberry completely occurs not in contact with to the position of antibacterial paper washer
It goes mouldy, and provided by the invention carry oily silver-colored zinc zeolite antibacterial paper washer and can persistently be released by contact sterilization and essential oil molecule simultaneously
It is put into inside food packaging in bottom clearance and plays bacteriostasis, preservation effect so that the red bayberry after the same terms storage does not go mouldy, and feels
Official is good.
2. carry the advantages of oily silver-colored zinc zeolite antibacterial paper washer combines silver-colored zinc zeolite and plants essential oil, performance is stable, antibacterial effect
Fruit is good.
Although there is a large amount of silver, zinc ion in the hole of silver-colored zinc zeolite inside, BET adsorption/desorptions are the experimental results showed that silver
Zinc zeolite still has substantial amounts of internal surface area (236.8769m2/ g), essential oil molecule can be largely adsorbed using these internal surface areas,
And without electrostatic force between essential oil molecule and zeolite, only by weaker dispersion force as adsorption capacity, convenient for the release of essential oil molecule.
The oily silver-colored zinc zeolite of load of the present invention is utilized respectively the hole that silver, zinc ion and essential oil are loaded into inside zeolite by electrostatic field and dispersion force
In gap, not only stability is good but also can play the advantages of essential oil release sterilization limits from contact area for manufactured antibacterial paper washer, comprehensive
The advantages of having closed the two.In addition the fungistatic effect of manufactured antibacterial paper washer gets a promotion after the zeolite-loaded essential oil of silver-colored zinc, to large intestine
The inhibition zone of bacillus, staphylococcus aureus and bacillus subtilis is respectively by 3.5 ± 0.3,3.5 ± 0.3,4.0 ± 0.3 (mm)
3.9 ± 0.2,3.7 ± 0.3,5.0 ± 0.2 (mm) are increased to, see Fig. 5 B.
(4) illustrate
Fig. 1 is that 1 step of embodiment (1) obtains the scanning electron microscope image of zeolite sample a, b, c, d, e, f, g (h is untreated
Zeolite).The solution treatment of different silver-colored zinc ratios has a certain impact to the pattern of zeolite so that particle surface generates part and lacks
It falls into, but not causes the extensive damage of zeolite granular.
Fig. 2 is the X-ray diffraction image of the zeolite sample before and after silver-colored zinc ion-exchange treatment, in scanning electron microscope image (figure
1) further demonstrating ion exchange and will not cause the extensive damage of zeolite unit cell on the basis of.And silver-colored zinc ion is
Entered by ion exchange in zeolitic frameworks.
Fig. 3 be silver-colored zinc zeolite (b) carry oil before and after scanning electron microscope image, silver-colored zinc zeolite b (a, b be respectively 1300 times and
5000 times of images) and silver-colored zinc zeolite b load cinnamaldehyde oil after (c, d are respectively 1300 times and 5000 times of images).
Fig. 4 is the surface for carrying oily silver-colored zinc zeolite antibacterial packing paper and the ethyl cellulose blank paper washer for not loading oily silver-colored zinc zeolite
And profile scanning microscopic comparison is as (from left to right：Appearance, section, surface).
Fig. 5 A are inhibition zone (Escherichia coli, staphylococcus aureus, the withered grass bud before and after silver-colored zinc zeolite (b) ultraviolet irradiation
Spore bacillus), show that silver-colored zinc zeolite (b) still has good bacteriostasis after ultraviolet irradiation is handled.1：Blank, 2：Silver-colored zinc
Zeolite b antibacterials paper washer (pre-irradiation), 3：Silver-colored zinc zeolite b antibacterials paper washer (254nm ultraviolet irradiation 4h are cycled 5 times).
Fig. 5 B are the inhibition zone images (by embodiment 2) for carrying oily silver-colored zinc zeolite, and after loading essential oil, bacteriostasis property further carries
It is high.1：Blank, 2：Silver-colored zinc zeolite antibacterial paper washer, 3：Carry oily silver-colored zinc zeolite antibacterial paper washer.
Fig. 5 C are to carry the result that oily silver-colored zinc zeolite inhibits aspergillus niger experiment (by embodiment 2).
Fig. 5 D are to carry the result that oily silver-colored zinc zeolite inhibits Penicillium citrinum experiment (by embodiment 2).After loading essential oil, to food table
The bacteriostasis property of the common Penicillium citrinum in face and aspergillus niger, which has, very significantly to be improved.
Fig. 6 A are the fresh-keeping effects that will carry oily silver-colored zinc zeolite antibacterial paper washer (being prepared by embodiment 2) applied to fresh Waxberry preservation
Fruit is schemed (after being stored 4 days at 4 DEG C).
Fig. 6 B are the principle schematics that the present invention carries oily silver-colored zinc zeolite antibacterial paper washer.Oily silver-colored zinc zeolite paper washer is carried to significantly improve
The shelf life of red bayberry, at the same carry oily silver-colored zinc zeolite paper washer compare do not carry oil silver-colored zinc zeolite paper washer antibacterial anti-corrosion effect it is more preferable.
(5) specific embodiment
Technical scheme is described further with specific embodiment below, but protection scope of the present invention is unlimited
In this：
Embodiment 1
(1) silver-colored zinc zeolite is prepared
By dry 5h at 100 DEG C of zeolite materials (purchased from Aladdin, 10 μm of average grain diameter), according to solid-to-liquid ratio 1 after cooling：10
(w/v) 100.0g zeolites are weighed to be separately added into prepared following solution：
(a)0.1mol·L-1Silver nitrate aqueous solution (1000mL)；
(b)0.1mol·L-1Silver nitrate solution (800mL) and 0.5molL-1The mixing of zinc nitrate solution (200mL) is molten
Liquid；
(c)0.1mol·L-1Silver nitrate solution (600mL) and 0.5molL-1The mixing of zinc nitrate solution (400mL) is molten
Liquid；
(d)0.1mol·L-1Silver nitrate solution (400mL) and 0.5molL-1The mixing of zinc nitrate solution (600mL) is molten
Liquid；
(e)0.1mol·L-1Silver nitrate solution (200mL) and 0.5molL-1The mixing of zinc nitrate solution (800mL) is molten
Liquid；
(f)0.5mol·L-1Zinc nitrate solution；
(g) distilled water；
It is sufficiently stirred scattered be placed in 60 DEG C of waters bath with thermostatic control and carries out ion exchange, taken out after keeping 10h with Medium speed filter paper
Decompression suction filtration is carried out, the silver ion into filtrate is at least rinsed with pure water with 0.1molL-1Sodium chloride solution is examined without apparent
White precipitate.Zeolite product of the flushing after qualified is transferred in glass dish and is placed in 70 DEG C of drying of convection oven overnight, after taking-up
Zeolite product is transferred in wide-mouth bottle to be placed at 70 DEG C of high-temperature vacuum baking oven and is dried in vacuo 2.5h.It is sealed after taking-up and uses aluminium foil
It is In Shade spare to wrap up body, it is a, b, c, d, e, f, g to mark sample respectively.
(2) resistance to discoloration test and inhibition zone test under ultraviolet irradiation accelerates
Weigh 2.0g ethyl celluloses and the above-mentioned zeolite samples being prepared of 100mg respectively, dissolving be scattered in 20mL without
In water-ethanol, after being sufficiently stirred at room temperature, coating liquid is obtained.According to 2mL/38.47cm2It is uniform that coating liquid pipettes quantitative coating liquid
Conventional absorbent paper paper surface is coated on, is protected from light natural drying at room temperature.Blank paper washer is prepared as without zeolite sample, simply by second
Base cellulose solution is coated on blotting paper, other processes are identical.Obtained paper washer containing zeolite sample is respectively designated as a, b, c,
D, e, f, g, blank are sampled using card punch and are carried out inhibition zone test, and remaining part carries out resistance to discoloration test.It is commented by combining
Valency, zeolite sample (b) be it is a kind of have good bacteriostasis property and it is ultraviolet accelerate it is not easy to change under irradiation, still select
Carrier of the silver-colored zinc zeolite (b) as essential oil.
(3) prepare and carry oily silver-colored zinc zeolite
It weighs 10.0g silver-colored zinc zeolites (b) and measures 5.0mL plants essential oils (cinnamic acid, carvacrol or Herba Origani Vulgaris quintessence oil) and burning
After being mixed in cup, sealed using sealed membrane and be placed on 2h (timing since being warming up to after 80 DEG C) in 90 DEG C of waters bath with thermostatic control, after 2h
It takes out, after being cooled to room temperature, after the free plants essential oil for carrying oily zeolite sample surface is quickly washed away using ether, obtains carrying oily silver
The sealing of zinc zeolite is kept in dark place.
The standard curve that cinnamic acid ethanol solution is first established under 305nm is：Y=5327.857x-3.571 × 10-5Take one
Quantitative sample (the silver-colored zinc zeolite of load cinnamic acid) measures its light absorption value, by following equation calculate 62.61%.
Cinnamic acid quality × 100% before quality/load of cinnamic acid in load factor (%)=zeolite
(4) prepare containing the oily silver-colored zinc zeolite coating liquid of load and antibacterial paper washer
2.0g ethyl celluloses and the above-mentioned load oil silver-colored zinc zeolites being prepared of 100mg are weighed respectively, and dissolving is scattered in
In 20mL absolute ethyl alcohols, after being sufficiently stirred at room temperature, obtain carrying the ethyl cellulose macromolecule half that oily silver-colored zinc zeolite uniformly disperses
Clear solution, this is to carry oily silver-colored zinc zeolite coating liquid.According to 2mL/38.47cm2Coating liquid pipettes quantitative coating liquid and uniformly applies
Conventional absorbent paper paper surface is distributed in, is protected from light natural drying at room temperature.This obtains carrying oily silver-colored zinc zeolite antibacterial paper washer.
Embodiment 2
By dry 4h at 100 DEG C of zeolite materials (purchased from Aladdin, 10 μm of average grain diameter), according to solid-to-liquid ratio 1 after cooling：10
(w/v) 100.0g zeolites are weighed and are separately added into prepared 0.1molL-1Silver nitrate solution (800mL) and 0.5molL-1Nitre
Scattered be placed in 60 DEG C of waters bath with thermostatic control is sufficiently stirred in the mixed solution of sour zinc solution (200mL) and carries out ion exchange, is kept
It is taken out after 10h and decompression suction filtration is carried out with Medium speed filter paper, the silver ion into filtrate is at least rinsed with pure water with 0.1molL-1
Sodium chloride solution is examined without apparent white precipitate.Zeolite product of the flushing after qualified is transferred in glass dish and is placed in convection oven
Zeolite product overnight, is transferred in wide-mouth bottle to be placed at 60 DEG C of high-temperature vacuum baking oven and is dried in vacuo 2h by 60 DEG C of drying after taking-up.
It is sealed after taking-up and In Shade spare with aluminium foil package body.
It weighs 10.0g silver-colored zincs zeolite and measures 6.0mL cinnamaldehyde oils and mixed (purchased from Aladdin, 95%) in beaker
Afterwards, 2h (timing since being warming up to after 80 DEG C) in 80 DEG C of waters bath with thermostatic control is placed on using sealed membrane sealing, is taken out after 2h, cooled down
To room temperature, after the free cinnamic acid for carrying oily zeolite sample surface is quickly washed away using ether, obtain carrying oily silver-colored zinc zeolite sealing
It is kept in dark place.
2.0g ethyl celluloses (purchased from Aladdin, molecular weight 246.30) are weighed respectively and 100mg is above-mentioned is prepared
Oily silver-colored zinc zeolite is carried, dissolving is scattered in 20mL absolute ethyl alcohols, after being sufficiently stirred at room temperature, is obtained carrying oily silver-colored zinc zeolite and uniformly be divided
The scattered translucent solution of ethyl cellulose macromolecule, this is to carry oily silver-colored zinc zeolite coating liquid.According to 2mL/38.47cm2Film
Liquid pipettes quantitative coating liquid and is spread evenly across conventional absorbent paper paper surface, is protected from light natural drying at room temperature.This obtains carrying oily silver-colored zinc
Zeolite antibacterial paper washer.
Embodiment 3
By dry 4h at 100 DEG C of zeolite materials (purchased from Aladdin, 10 μm of average grain diameter), according to solid-to-liquid ratio 1 after cooling：10
(w/v) 100.0g zeolites are weighed and are separately added into prepared 0.1molL-1Silver nitrate solution (800mL) and 0.5molL-1Nitre
Scattered be placed in 60 DEG C of waters bath with thermostatic control is sufficiently stirred in the mixed solution of sour zinc solution (200mL) and carries out ion exchange, is kept
It is taken out after 12h and decompression suction filtration is carried out with Medium speed filter paper, the silver ion into filtrate is at least rinsed with pure water with 0.1molL-1
Sodium chloride solution is examined without apparent white precipitate.Zeolite product of the flushing after qualified is transferred in glass dish and is placed in convection oven
Zeolite product overnight, is transferred in wide-mouth bottle to be placed at 60 DEG C of high-temperature vacuum baking oven and is dried in vacuo 2h by 60 DEG C of drying after taking-up.
It is sealed after taking-up and In Shade spare with aluminium foil package body.
It weighs 5.0g silver-colored zincs zeolite and measures after 3.6mL cinnamaldehyde oils mix (purchased from Aladdin, 95%) in beaker,
2h (timing since being warming up to after 80 DEG C) in 80 DEG C of waters bath with thermostatic control is placed on using sealed membrane sealing, takes out, is cooled to after 2h
After room temperature, after the free cinnamic acid for carrying oily zeolite sample surface is quickly washed away using ether, obtain carrying oily silver-colored zinc zeolite sealing and keep away
Light preserves.
2.0g ethyl celluloses (purchased from Aladdin, molecular weight 246.30) are weighed respectively and 100mg is above-mentioned is prepared
Oily silver-colored zinc zeolite is carried, dissolving is scattered in 20mL absolute ethyl alcohols, after being sufficiently stirred at room temperature, is obtained carrying oily silver-colored zinc zeolite and uniformly be divided
The scattered translucent solution of ethyl cellulose macromolecule, this is to carry oily silver-colored zinc zeolite coating liquid.According to 2mL/38.47cm2Film
Liquid pipettes quantitative coating liquid and is spread evenly across conventional absorbent paper paper surface, is protected from light natural drying at room temperature.This obtains carrying oily silver-colored zinc
Zeolite antibacterial paper washer.
Silver-colored zinc zeolite sample prepared by embodiment 1 is carried out X-ray energy spectrum analysis (EDX) measure silver-colored zinc ion therein and
Dissociated ion content, analysis result are shown in Table 1.Wherein zeolite sample (b) has higher silver-colored zinc ion concentration.
Metal ion content analysis result in 1 each zeolite sample of table
(a)0.1mol Ag+,(b)0.08mol Ag+and 0.1mol Zn2+,(c)0.06mol Ag+and 0.2mol
Zn2+,(d)0.04mol Ag+and 0.3mol Zn2+,(e)0.02mol Ag+and 0.4mol Zn2+,(f)0.5mol Zn2+,
(g) Purified water, (h) are untreated；ND, expression do not detect
Inhibition zone measure is carried out to silver-colored zinc zeolite sample prepared by embodiment 1, as a result such as table 2, zeolite sample (b) have compared with
Good bacteriostasis property.
The inhibition zone of 2 each zeolite sample of table measures
Inhibition zone is not observed in NA expressions
The coating paper washer of each zeolite sample is subjected to resistance to discoloration evaluation, with 254nm ultraviolet irradiation 4h, is taken out after cycling 5 times,
It is measured with colour difference meter.
3 resistance to discoloration test result of table
UV represents ultraviolet irradiation processing, L*, a*, b*It is measured four times, is averaged with colour difference meter respectively.
It is evaluated by Hunter (Hunter) whiteness formulas and aberration total value Δ E.The result shows that although silver zeolite (a)
It is easily graying under ultraviolet irradiation, but substantially improve its discoloration-resistant performance after introducing zinc ion.For bacteriostasis property and resistance to discoloration
Performance considers, and it is suitable to select silver-colored zinc zeolite (b) as the carrier of essential oil.
Claims (7)
- A kind of 1. silver-colored zinc zeolite antibacterial paper washer for loading plants essential oil, which is characterized in that the silver-colored zinc boiling of the load plants essential oil Stone antibacterial paper washer is prepared as follows obtaining：(1) silver-colored zinc zeolite is preparedZeolite materials are placed at 80~100 DEG C dry 4~6h, according to solid-to-liquid ratio 1 after being cooled to room temperature：10~12 add in silver-colored zinc In mixed solution, be dispersed with stirring and be placed at 40~60 DEG C 8~12h of heat preservation, after through filtering, washing, filtration cakes torrefaction, obtain silver Zinc zeolite；(2) prepare and carry oily silver-colored zinc zeoliteSilver-colored zinc zeolite obtained by step (1) is mixed with plants essential oil, sealing is placed on heat preservation 2~4h, Zhi Houleng at 80~100 DEG C But to room temperature, washed with ether, obtain carrying oily silver-colored zinc zeolite；The volumetric usage of the plants essential oil is calculated as 0.5~0.75mL/g with the quality of silver-colored zinc zeolite；(3) the silver-colored zinc zeolite antibacterial paper washer of load plants essential oil is preparedOily silver-colored zinc zeolite will be carried obtained by ethyl cellulose, step (2) to add in absolute ethyl alcohol, is dispersed with stirring uniformly, is obtained at room temperature To coating liquid, gained coating liquid is spread evenly across blotting paper surface, is protected from light natural drying at room temperature to get the load plant The silver-colored zinc zeolite antibacterial paper washer of essential oil；The oily silver-colored zinc zeolite and the mass ratio of ethyl cellulose of carrying is 1：10~20；The volumetric usage of the absolute ethyl alcohol is calculated as 50~200mL/g to carry the quality of oily silver-colored zinc zeolite.
- 2. the silver-colored zinc zeolite antibacterial paper washer of load plants essential oil as described in claim 1, which is characterized in that in step (1), institute The preparation method for stating silver-colored zinc mixed solution is：By 0.1mol/L silver nitrate solutions and 0.5mol/L zinc nitrate solutions by volume 1： 0.25~4 mixing to get.
- 3. the silver-colored zinc zeolite antibacterial paper washer of load plants essential oil as described in claim 1, which is characterized in that in step (1), institute It states suction filtration and decompression suction filtration is carried out with Medium speed filter paper.
- 4. the silver-colored zinc zeolite antibacterial paper washer of load plants essential oil as described in claim 1, which is characterized in that in step (1), institute It states washing to be rinsed with pure water, and rinses to the silver ion in filtrate and examined with 0.1mol/L sodium chloride solutions without apparent Until white precipitate.
- 5. the silver-colored zinc zeolite antibacterial paper washer of load plants essential oil as described in claim 1, which is characterized in that in step (1), institute Stating dry method is：Dry 10~12h will be placed in 60~80 DEG C of convection oven by the filter cake of washing, be then placed in again Dry 2~3h in 60~80 DEG C of vacuum drying oven, finally takes out and is kept in dark place in shady place sealing.
- 6. the silver-colored zinc zeolite antibacterial paper washer of load plants essential oil as described in claim 1, which is characterized in that in step (2), institute Plants essential oil is stated as cinnamic acid, carvacrol or Herba Origani Vulgaris quintessence oil.
- 7. the silver-colored zinc zeolite antibacterial paper washer of load plants essential oil as described in claim 1, which is characterized in that in step (3), institute The coating method for stating coating liquid is：Coating liquid is evenly applied to blotting paper surface using Meyer stick, coating weight for 0.05~ 0.06mL/cm2, volatilize and dry naturally.
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