CN105038090B - A kind of preparation method of antibacterial electronic cigarette appearance material - Google Patents
A kind of preparation method of antibacterial electronic cigarette appearance material Download PDFInfo
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Abstract
The invention provides a kind of novel antibacterial electronic cigarette appearance material and preparation method thereof.For the present invention using tetraethyl orthosilicate and sodium metaaluminate as raw material, water is solvent, and under the template action of tripropyl ammonium hydroxide and tripropyl ammonium bromide, by molecular self-assembling, the nanometer sial zeolitic material with microcellular structure is prepared.The nanometer micropore zeolite obtains silver-carrying nano zeolite by soaking silver nitrate solution after high-temperature calcination.Silver-carrying nano zeolite with carrying silver surface is after the modification that organises, it is added to by melt-blending process in polyethylene (PE), polypropylene (PP), butadiene acrylonitrile styrene resin (ABS), nano silver-carrying zeolite/plastics composite antibacterial material is made.The anti-biotic material raw material of the present invention is simple and easy to get, mature technical route, can be used as a kind of new antibacterial electronic cigarette shell material, during electronic cigarette Reusability, plays antibacterial effect, prevents bacteria breed infringement electronic cigarette user's health.
Description
Technical field
The invention belongs to electronic cigarette Material Field, is a kind of preparation method of novel antibacterial electronic cigarette appearance material.
Background technology
Antibacterial functionalized technology and its product are that people propagate and advanced in living standard huge to prevention disease in recent years
Under big requirement drive, the new technology and new product that are developed rapidly.Electronic cigarette is a kind of product of Reusability, usual electronics
The other plastics of technical grade of cigarette appearance material use, resin antibiotic property are poor, for a long time using easy breed bacteria, influence to use
The health of person.Antiseptic is added in the plastic, is bred so that the bacterium for sticking in smoke pipe surface is killed or resisted within a certain period of time,
Modified smoke pipe material is by with excellent anti-microbial property.Application technology exploitation of the antiseptic in plastic products is increasingly pasted
The manufacturing requirements of nearly user's product, has all been obtained in fields such as pipeline material, daily washing machine, refrigerator, medical supplies
Application, but there is presently no the plastic applications with excellent anti-bacterium capability in electronic cigarette appearance material field.
The core of antibiotic plastic is antiseptic, also referred to as antimicrobial powder.The antimicrobial powder of synthesis is divided into organic anti-bacterial
Powder and the major class of inorganic antibiosis powder two.The problem of organic anti-bacterial powder is due to heat endurance, antibiotic plastic field apply compared with
It is few.Inorganic antibiosis powder is divided into silicate (including zeolite, Tuo Bo are established and come stone, silica gel glass, bentonite etc.), phosphorus from carrier
Phosphate-gallate series (including basic zirconium phosphate, calcium phosphate etc.), oxide system (including TiO2、ZrO2、Al2O3Deng) and other (such as activated carbon, carbon
Fiber, complex compound etc.).Silver system can be divided into according to the active ingredient of antiseptic and (contain Ag+、Cu2+、Zn2+Deng metal ion) and titanium system
(there is the TiO of photocatalysis2Deng) antiseptic：Carry silver-colored silicate antiseptic and be mainly used in the fiber of low temperature process, plastics
Deng product, carry the phosphate-based antiseptic of silver and oxide photocatalyst series antibacterial agent is mainly used in the ceramic product of high temperature process.Mesh
The development of preceding antiseptic focuses on developing new carrier, if Zhoushan Tomorrow Nanomaterials Co., Ltd is in Publication No.
A kind of nano silicon-based oxide Ag-carried antibacterial powder is disclosed in CN1344494 application for a patent for invention.Shanghai Normal University is in public affairs
The number of opening is a kind of silver-carried antibacterial agent with nanometer porous disclosed in CN1817138 application for a patent for invention.Xiamen University is in Publication No.
A kind of preparation method of silver supported ammonium modified nano zeolite antibacterial agent disclosed in CN1919000A application for a patent for invention.
The content of the invention
It is an object of the invention to provide a kind of preparation method of novel antibacterial electronic cigarette appearance material, specially one kind is received
The preparation method of rice zeolite with carrying silver/plastic composite, the material obtained can be made into the electronic cigarette sleeve pipe of excellent antibacterial performance.
Major defect one existing for existing carrying silver antimicrobials is that silver ion is unstable, in sunlight or the feelings of heating
The outward appearance of elemental silver and coloured effect product is easily reduced under condition, second, for silicate such as Ag Loaded Zeolite Antimicrobial by
It is mainly inorganic component in it, is not easy to form uniform blocks in the cohesive process with plastics, influences the outward appearance and performance of product.
In order to obtain excellent antibacterial performance and not influence the electronic cigarette sleeve pipe composite of plastics performance itself, the present invention prepares nanometer chi
Very little zeolite micropore material is effectively to accommodate silver ion.Therefore employ in technical scheme and continuously stir the method for heating to obtain
The carrier of Nano grade.The Ag-carried antibacterial material of report different from the past, use ultrasonic disperse in the present invention, the method for backflow with
And organo-functionalization modification is carried out to nano silver-carrying zeolite using the agent of silane idol makes it form more homogeneous composite wood with plastics
Material.
Nano zeolite carrier provided by the invention is crystalline material, has the size of nanosized.Using electron microscope
The microscopic appearance of zeolite powder is observed, the grain diameter of zeolite powder be 30~50nm, and particle size distribution is more uniform (schemes
1).The zeolite powder of gained has microcellular structure, by nitrogen adsorption isotherm measure come pore size be aboutCompare table
Area is 358m2/ g, pore volume 0.06cm3·g-1, it is sufficient to accommodate the silver ion (Fig. 2) with fungistatic effect.Load silver ion
Nano material afterwards is declined slightly to 344m than surface2/ g, illustrate that silver ion has successfully loaded the duct (figure into nano zeolite
3).Because nano-particle has a nanometer size effect and skin effect, the zeolitic material of the type is as carrier, favorably
In the load capacity of increase silver ion.The nano zeolite infrared spectrum being modified by organo-functionalization is shown in Fig. 4, due to 1275 Hes
2900cm-1The outer characteristic absorption peak of the two silane couplers of wave number overlaps with the infrared absorption peak of zeolitic material, it is impossible to bright
It is aobvious to observe, but still can see 1735cm-1There is the absworption peak of silane coupler at place, and this peak is in the zeolitic material not organised
In be no, show that silane coupler is successfully linked on Target Zeolite material.Carry silver-colored front and rear and organo-functional group
The thermogravimetric analysis (Fig. 5) of nano zeolite after changing before modified, shows that the zeolite heat endurance after silane coupled is higher.It is organic
The modified nano zeolite of function dough is preferably combined with the plastics of macromolecule composition, can reach 5% addition without shadow
Ring the outward appearance and performance of electronic cigarette shell material.
The present invention proposes novel antibacterial electronic cigarette appearance material, it is characterised in that it is made up of silver-carrying nano zeolite and plastics,
Cubage by mass percentage, zeolite containing silver-carrying nano are 1%~5%, are 95%~99% containing plastics.
Invention also provides a kind of above-mentioned preparation method of novel antibacterial electronic cigarette appearance material, it is characterised in that bag
Include following steps：
(1) zeolite that particle is Nano grade is prepared：By TPAOH (TPAOH) and sodium metasilicate (NaAlO2)
Stirring and dissolving adds in water or is not added with 4-propyl bromide (TPABr), after being stirred at room temperature 10~50 minutes, obtains uniformly
Mixed solution, add tetraethyl orthosilicate (TEOS) be stirred at room temperature overnight；Gained mixture is in 130 DEG C of -150 DEG C of oil baths
Reaction, is washed respectively after centrifugation with water and ethanol, and target nanosized zeolitic material is obtained after 60-70 DEG C of drying.
(2) silver-carrying nano zeolite is prepared：After step 1 gained nano zeolite vacuum is calcined into the organic amine removed in duct,
It is scattered in silver nitrate (AgNO3) in the aqueous solution, lucifuge stirring, after product is washed with deionized, drying, silver-carrying nano boiling is made
Stone material.
(3) organic modification is carried out to nano zeolite：Step 2 silver-carrying nano zeolite is divided in alcohol-water mixed solution
Dissipate, add silane coupler KH570 and a small amount of acetic acid, be heated to reflux, it is 7 to be washed with distilled water to pH value, then uses absolute ethyl alcohol
Wash, 10-15 hours are dried in vacuo at 60-70 DEG C, obtain the nanosized zeolitic material of organic modification.
(4) silver-carrying nano zeolite/plastic composite is prepared：By polyethylene (PE) or polypropylene (PP) or butadiene-the third
Alkene nitrile-styrene resin (ABS) plastic master batch heating melting, the nano silver-carrying zeolite antibacterial agent of organic modification is by 1~5%
Mass fraction adds blended under agitation in melt, and nano silver-carrying zeolite/plastic composite is made using tablet press machine.
Currently preferred technical scheme is：
In step 1, by the way of heating is continuously stirred, magnetic stirring speed is 250~400 revolutions per minute for described reaction
Clock, time are 12~72 hours.
Gained Zeolite is 2.95 in step 1, and granular size is 30~50nm, and nitrogen adsorption is than surface
358m2·g-1, aperture isPore volume is 0.06cm3·g-1。
Step 1 gained nano zeolite is used in 200 DEG C of vacuum in step 2 and is calcined 3~5 hours, adds 0.01~0.10M
AgNO3Solution, magnetic agitation 5~12 hours.
It is 1.3% that the nanosized zeolitic material of the organic modification, which carries silver-colored weight/mass percentage composition, carries nitrogen adsorption ratio after silver
Surface is 344m2·g-1。
It is described be heated to reflux after adding KH570, to be returned in water and the mixed solution of ethanol using ultrasonic disperse in step 3
Stream 30 minutes.
Nano zeolite infrared line after organic modification is in 1700cm-1There are obvious absorption peaks at place, and the absworption peak is silane
Characteristic peak.
Preferred technical scheme of the invention comprises the following steps that：
(1) zeolite that particle is Nano grade is prepared：By TPAOH (TPAOH) and sodium metasilicate (NaAlO2)
Stirring and dissolving adds in water or is not added with 4-propyl bromide (TPABr), after being stirred at room temperature 10~50 minutes, obtains uniformly
Mixed solution, add tetraethyl orthosilicate (TEOS) be stirred at room temperature overnight, TEOS:NaAlO2:TPAOH:TPABr:H2O's
Mol ratio is 20~30:1:3~9:0~5:1000.Gained mixture is in 140 DEG C of oil baths with 250~400 rpms of speed
Degree continuously stirs heating 12~72 hours, washes twice the above respectively with water and ethanol after centrifugation, mesh is obtained after 70 DEG C of drying
Mark nanosized zeolitic material.
(2) nano zeolite for carrying silver is prepared：Step 1 gained nano zeolite is calcined 3~5 hours in 200 DEG C of vacuum and removed
After removing the organic amine in duct, 0.01M silver nitrate (AgNO is scattered in3) solution, lucifuge stirring, product is washed with deionized
Afterwards, dry, silver-carrying nano zeolitic material is made.
(3) organic modification is carried out to nano zeolite：Step 2 silver-carrying nano zeolite is divided in alcohol-water mixed solution
Dissipate, add silane coupler KH570 and a small amount of acetic acid, regulation pH value is 2~3, is heated to reflux 30min, is washed with distilled water to
PH value is 7, then is washed for several times with absolute ethyl alcohol, is dried in vacuo 12 hours at 70 DEG C.Obtain the nanosized zeolitic material of organic modification.
(4) nano silver-carrying zeolite/plastic composite is prepared：By polyethylene (PE) or polypropylene (PP) or butadiene-the third
Alkene nitrile-styrene resin (ABS) plastic master batch heating melting, the nano silver-carrying zeolite antibacterial agent of organic modification press 1% and 5%
Mass fraction adds blended under agitation in melt, and making nano silver-carrying zeolite/plastic composite using tablet press machine surveys tentative standard
Test specimen.
The present invention proposes a kind of preparation method of new Nano Silver carrier and antimicrobial composite material.Report different from the past
The phosphate support in road, present invention employs new zeolite micropore material to do carrier, and the material has micropore size and pore volume,
Silver ion can effectively be accommodated.Employed in invention and continuously stir the method for heating to obtain the Zeolite support of Nano grade and adopt
With ultrasonic disperse, the method for backflow carries out organo-functionalization modification to nano silver-carrying zeolite using the agent of silane idol makes itself and plastics
Form more homogeneous composite.The composite raw material of the present invention is simple and easy to get, will have for electronic cigarette outward appearance anti-biotic material
There is extensive market application foreground.
Brief description of the drawings
Fig. 1 is that the TEM of nano zeolite of the present invention schemes.
The nitrogen adsorption isotherm of nano zeolites of the Fig. 2 for present invention load before silver-colored.
The nitrogen adsorption isotherm of nano zeolites of the Fig. 3 for present invention load after silver-colored.
Fig. 4 is the infrared spectrum of the silane coupled front and rear nano zeolite of the present invention.
The thermogravimetric analysis figure of nano zeolites of the Fig. 5 for present invention load before and after silver-colored.
Embodiment
Embodiment 1：By 1.016g TPAOHs (TPAOH) and 0.082g sodium metasilicates (NaAlO2) stirring and dissolving
In 12mL water, 1.065g 4-propyl bromides (TPABr) are dissolved in 6mL water, the mixing of two kinds of solution, through be stirred at room temperature 10~
After 50 minutes, uniform solution is obtained, tetraethyl orthosilicate (TEOS) 4.792g is added and is stirred at room temperature overnight.Gained mixture
Heating 12 hours is continuously stirred with 250 rpms of speed in 140 DEG C of oil baths, washed respectively with water and ethanol after centrifugation
Wash more than twice, target nanosized zeolitic material is obtained after 70 DEG C of drying.After gained nano zeolite is calcined 5 hours in 200 DEG C of vacuum,
It is scattered in 0.01M silver nitrate (AgNO3) aqueous solution 50mL, lucifuge stirring 12h, after product is washed with deionized, dry, system
Obtain silver-carrying nano zeolitic material.Alcohol-water mixed solution (volume ratios 1 of the gained silver-carrying nano zeolite 500mg in 20mL:1) in
It is scattered, 1mL silane couplers KH570 and a small amount of acetic acid are added, regulation pH value is 3, is heated to reflux 30min, with distillation water washing
It is 7 to pH value, then is washed for several times with absolute ethyl alcohol, is dried in vacuo 12 hours at 70 DEG C.Obtain the nano zeolite material of organic modification
Material.By the 180 DEG C of heating meltings of 55g ABS plastic master batch, the nano silver-carrying zeolite antibacterial agent 500mg of organic modification adds melt
Interior blended under agitation, nano silver-carrying zeolite/plastic composite test standard specimen is made using tablet press machine.
Embodiment 2：By 1.531g TPAOHs (TPAOH) and 0.083g sodium metasilicates (NaAlO2) stirring and dissolving
In 18mL water, after being stirred at room temperature 10~50 minutes, uniform mixed solution is obtained, adds tetraethyl orthosilicate (TEOS)
5.125g it is stirred at room temperature overnight.Gained mixture continuously stirs heating in 140 DEG C of oil baths with 250 rpms of speed
72 hours, the above was washed twice respectively with water and ethanol after centrifugation, target nanosized zeolitic material is obtained after 70 DEG C of drying.Nanometer
Zeolite carries silver, organises, prepares composite step with embodiment 1 with plastic molten melt blending.
Embodiment 3：By 1.039g TPAOHs (TPAOH) and 0.078g sodium metasilicates (NaAlO2) stirring and dissolving
In 18mL water, add 0.089g 4-propyl bromides (TPABr), after being stirred at room temperature 10~50 minutes, uniformly mixed
Solution, add tetraethyl orthosilicate (TEOS) 4.167g and be stirred at room temperature overnight.Gained mixture is in 140 DEG C of oil baths with 400
Rpm speed continuously stir heating 24 hours, wash twice the above respectively with water and ethanol after centrifugation, 70 DEG C of bakings
Target nanosized zeolitic material is obtained after dry.Loading Nanoscaled Zeolite Composited silver, organise, composite step is prepared with plastic molten melt blending with real
Apply example 1.
Embodiment 4：By 1.827g TPAOHs (TPAOH) and 0.085g sodium metasilicates (NaAlO2) stirring and dissolving
In 18mL water, after being stirred at room temperature 10~50 minutes, uniform mixed solution is obtained, adds tetraethyl orthosilicate (TEOS)
6.240g it is stirred at room temperature overnight.Gained mixture continuously stirs heating in 140 DEG C of oil baths with 400 rpms of speed
24 hours, the above was washed twice respectively with water and ethanol after centrifugation, target nanosized zeolitic material is obtained after 70 DEG C of drying.Nanometer
Zeolite carries silver, organises, prepares composite step with embodiment 1 with plastic molten melt blending.
Embodiment 5：After gained nano zeolite is calcined 5 hours in 200 DEG C of vacuum in embodiment 1,50mL is scattered in
0.10M silver nitrate (AgNO3) aqueous solution, lucifuge stirring 12h, after product is washed with deionized, drying, silver-carrying nano is made
Zeolitic material.Silver-carrying nano zeolite organises, prepares composite step with embodiment 1 with plastic molten melt blending.
Embodiment 6：The nanosized zeolitic material preparation method of organic modification is the same as embodiment 1.By 55g ABS plastic master batches
180 DEG C of heating meltings, the nano silver-carrying zeolite antibacterial agent 2.50g of organic modification add blended under agitation in melt, utilize tabletting
Mechanism makees nano silver-carrying zeolite/plastic composite test standard specimen.
Embodiment 7：The nanosized zeolitic material preparation method of organic modification is the same as embodiment 1.By 45g PP plastic master batches 120
DEG C heating melting, the nano silver-carrying zeolite antibacterial agent 500mg of organic modification add blended under agitation in melt, utilize tabletting mechanism
Make nano silver-carrying zeolite/plastic composite test standard specimen.
Embodiment 8：The nanosized zeolitic material preparation method of organic modification is the same as embodiment 1.By 45g PE plastic master batches 120
DEG C heating melting, the nano silver-carrying zeolite antibacterial agent 500mg of organic modification add blended under agitation in melt, utilize tabletting mechanism
Make nano silver-carrying zeolite/plastic composite test standard specimen.
Claims (8)
1. a kind of preparation method of antibacterial electronic cigarette appearance material, it is characterised in that comprise the following steps：
(1) zeolite that particle is Nano grade is prepared：By TPAOH (TPAOH) and sodium metaaluminate (NaAlO2) stirring
It is dissolved in water, adds 4-propyl bromide (TPABr), after being stirred at room temperature 10~50 minutes, obtain uniform mixed solution,
Tetraethyl orthosilicate (TEOS) is added to be stirred at room temperature overnight；Gained mixture reacts in 130 DEG C of -150 DEG C of oil baths, centrifugation point
Washed respectively with water and ethanol from rear, target nanosized zeolitic material is obtained after 60-70 DEG C of drying；
(2) silver-carrying nano zeolite is prepared：After step 1 gained nano zeolite vacuum is calcined into the organic amine removed in duct, disperse
In silver nitrate (AgNO3) in the aqueous solution, lucifuge stirring, after product is washed with deionized, drying, silver-carrying nano zeolite material is made
Material；
(3) organic modification is carried out to nano zeolite：Step 2 silver-carrying nano zeolite is disperseed in alcohol-water mixed solution, added
Enter silane coupler KH570 and a small amount of acetic acid, be heated to reflux, it is 7 to be washed with distilled water to pH value, then is washed with absolute ethyl alcohol,
10-15 hours are dried in vacuo at 60-70 DEG C, obtain the nanosized zeolitic material of organic modification；
(4) silver-carrying nano zeolite/plastic composite is prepared：By polyethylene (PE) or polypropylene (PP) or butadiene-acrylonitrile-
The heating melting of styrene resin (ABS) plastic master batch, the nano silver-carrying zeolite antibacterial agent of organic modification press 1~5% quality
Fraction adds blended under agitation in melt, and nano silver-carrying zeolite/plastic composite is made using tablet press machine.
2. the preparation method of antibacterial electronic cigarette appearance material according to claim 1, it is characterised in that described in step 1
Reaction using heating is continuously stirred by the way of, magnetic stirring speed be 250~400 rpms, the time be 12~72 hours.
3. the preparation method of antibacterial electronic cigarette appearance material according to claim 1, it is characterised in that gained boils in step 1
Stone silica alumina ratio is 2.95, and granular size is 30~50nm, and nitrogen adsorption is 358m than surface2·g-1, aperture isPore volume is
0.06cm3·g-1。
4. the preparation method of antibacterial electronic cigarette appearance material according to claim 1, it is characterised in that by step in step 2
1 gained nano zeolite uses to be calcined 3~5 hours in 200 DEG C of vacuum, adds 0.01~0.10M AgNO3Solution, magnetic agitation 5
~12 hours.
5. the preparation method of antibacterial electronic cigarette appearance material according to claim 1, it is characterised in that described organise changes
Property nanosized zeolitic material to carry silver-colored weight/mass percentage composition be 1.3%, it is 344m to carry after silver nitrogen adsorption than surface2·g-1。
6. the preparation method of antibacterial electronic cigarette appearance material according to claim 1, it is characterised in that described in step 3
Be heated to reflux after adding KH570, being flowed back 30 minutes in water and the mixed solution of ethanol using ultrasonic disperse.
7. the preparation method of antibacterial electronic cigarette appearance material according to claim 1, it is characterised in that after organic modification
Nano zeolite infrared line in 1700cm-1There are obvious absorption peaks at place, and the absworption peak is the characteristic peak of silane.
8. according to the preparation method of any described antibacterial electronic cigarette appearance material in claim 1-7, it is characterised in that including
Following steps：
(1) zeolite that particle is Nano grade is prepared：By TPAOH (TPAOH) and sodium metaaluminate (NaAlO2) stirring
It is dissolved in water, adds 4-propyl bromide (TPABr), after being stirred at room temperature 10~50 minutes, obtain uniform mixed solution, add
Enter tetraethyl orthosilicate (TEOS) to be stirred at room temperature overnight, TEOS:NaAlO2:TPAOH:TPABr:H2O mol ratio be 20~
30:1:3~9:0~5:1000.Gained mixture is continuously stirred in 140 DEG C of oil baths with 250~400 rpms of speed to be added
Heat 12~72 hours, the above is washed twice respectively with water and ethanol after centrifugation, target nano zeolite material is obtained after 70 DEG C of drying
Material；
(2) nano zeolite for carrying silver is prepared：Step 1 gained nano zeolite is calcined 3~5 hours in 200 DEG C of vacuum and removes hole
After organic amine in road, 0.01M silver nitrate (AgNO is scattered in3) solution, lucifuge stirring, after product is washed with deionized,
Drying, silver-carrying nano zeolitic material is made；
(3) organic modification is carried out to nano zeolite：Step 2 silver-carrying nano zeolite is disperseed in alcohol-water mixed solution, added
Enter silane coupler KH570 and a small amount of acetic acid, regulation pH value is 2~3, is heated to reflux 30min, being washed with distilled water to pH value is
7, then washed for several times with absolute ethyl alcohol, it is dried in vacuo 12 hours at 70 DEG C；Obtain the nanosized zeolitic material of organic modification；
(4) nano silver-carrying zeolite/plastic composite is prepared：By polyethylene (PE) or polypropylene (PP) or butadiene-acrylonitrile-
The heating melting of styrene resin (ABS) plastic master batch, the nano silver-carrying zeolite antibacterial agent of organic modification is by 1%-5% mass point
Number adds blended under agitation in melt, and nano silver-carrying zeolite/plastic composite is made using tablet press machine.
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| CN109265819A (en) * | 2018-08-09 | 2019-01-25 | 道晟拉链科技（太仓）有限公司 | A kind of slide fastener coupling element antibiotic plastic and preparation method thereof |
| CN110254014B (en) * | 2019-03-19 | 2021-07-30 | 三菱电机(中国)有限公司 | Efficient antibacterial ABS plastic and preparation method thereof |
| CN110204828A (en) * | 2019-06-11 | 2019-09-06 | 温州医科大学附属口腔医院 | A kind of dental filling chock |
| CN113292333A (en) * | 2021-06-24 | 2021-08-24 | 四川三联新材料有限公司 | Preparation method of silver-loaded hydroxyapatite atomization core |
| CN115418071A (en) * | 2022-08-16 | 2022-12-02 | 宁波坚锋新材料有限公司 | Antibacterial ABS composite material and preparation method thereof |
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