CN105256536A - Preparation method for improved electronic cigarette flocculent filler fiber - Google Patents
Preparation method for improved electronic cigarette flocculent filler fiber Download PDFInfo
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- CN105256536A CN105256536A CN201510782497.1A CN201510782497A CN105256536A CN 105256536 A CN105256536 A CN 105256536A CN 201510782497 A CN201510782497 A CN 201510782497A CN 105256536 A CN105256536 A CN 105256536A
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Abstract
The invention discloses a preparation method for improved electronic cigarette flocculent filler fiber, and particularly provides a method for preparing improved electronic cigarette flocculent filler fiber through antibacterial substances and mesoporous materials. Electronic cigarette flocculent substances which have the antibacterial property and high adsorption/desorption capacity are finally obtained mainly by arranging antibacterial agents with phenolic groups on the surfaces of fiber through oxidation polymerization, conducting connection through coupling agents and adding mesoporous materials to the flocculent substances. The preparation method is simple and reliable, prepared electronic cigarette flocculent filler has rough surfaces, a large number of mesoporous materials are adsorbed to the surfaces, the adsorption/desorption performance is enhanced, and the antibacterial performance is good.
Description
Technical field
The invention belongs to electronic cigarette field of material technology, particularly relate to the method for modifying of the electronic cigarette floccule of a kind of rough porous surface and antibiotic property.
Background technology
Electronic cigarette is a kind of product electronic cigarette solution being transmitted nicotine or other materials through atomizer atomization to respiratory system.The cotton-shaped filler of electronic cigarette is the part storing tobacco tar in electronic cigarette, all has important impact for the tobacco tar content in an electronic cigarette, reliability, mouthfeel.Require there is the attached performance of good adsorption/desorption to materials such as nicotine, solvent, essence and flavoring agents in tobacco tar, be in use not easy breed bacteria, and can be high temperature resistant.
At present, the cotton-shaped filler material of main part in electronic cigarette comprises polyester fiber, acid fiber by polylactic, cellulose, nylon, polypropylene fibre, polyurethane foam post, polypropylene expanded post, micropore ceramics, foam metal material.These materials possess good hot property, and reliability is higher, but antibiotic property and the attached performance of adsorption/desorption do not need to improve these fibers itself.Cotton-shaped filler fiber surface modification is not strengthened to the effective ways of its antibiotic property and the attached performance of adsorption/desorption at present.The present invention proposes a kind of with the method on organic aldehydes matter and mesoporous material modified fibre surface, organic phenols substance improves the antibiotic property of fiber enough effectively, and increases the roughness of fiber surface; Mesoporous material is then for fiber provides the good attached performance of adsorption/desorption.
Summary of the invention
The object of the present invention is to provide the method for modifying of the cotton-shaped filler fiber of a kind of electronic cigarette, by fiber surface grafting antibacterial material and mesoporous material, improve its antibiotic property and the attached performance of adsorption/desorption.
The present invention is realized by the following technical programs:
A preparation method for the cotton-shaped filler fiber of modification electronic cigarette, is characterised in that, comprises the following steps:
Step one: cotton-shaped filler fiber is first used organic solvent washing, then in water Ultrasonic Cleaning;
Step 2: cotton-shaped filler fiber is transferred in antimicrobial, takes out after complete reaction;
Step 3: cotton-shaped filler fiber is transferred in the solution containing difunctional coupling agent, takes out after complete reaction;
Step 4: cotton-shaped filler fiber and the mesoporous material containing active end group are reacted in organic inert solvent, obtains the cotton-shaped filler fiber of modification electronic cigarette with antibiotic property and high adsorption/desorption ability after complete reaction.
Further improvement, in described step 2, antiseptic is organic phenolic antiseptic; Described organic phenolic antiseptic is any one or more than one mixing in 4-(2-amino-ethyl)-1,2-benzenediol, 3,4-dihydroxyphenyl-L-alanine, amino-1, the 2-catechol of 4-.
Further improvement, the concentration of described organic phenolic antiseptic is 1-5mg/mL.
Further improvement, in described step 2, the solvent of antimicrobial is water, adopts trishydroxymethylaminomethane to be that buffer regulates antimicrobial pH to 7-9.
Further improvement, in described step 3, difunctional coupling agent is any one in difunctional epoxy resin, difunctional isocyanates, difunctional acid anhydrides.
Further improvement, in described step 3, the concentration of described difunctional coupling agent is 5-10mg/ml.
Further improvement, in described step 4, mesoporous material is obtained by sol-gal process, and mesoporous material is carbon back mesoporous material or silicon-based mesoporous material.
Further improvement, in described step 4, carbon back mesoporous material with amphipathic nature block polymer be template, resol for matrix obtain; Silicon-based mesoporous material with amphipathic nature block polymer be template, ethyl orthosilicate for matrix obtain.
Further improvement, in described step 4, silicon-based mesoporous material suspension concentration is 10-15mg/ml
Further improvement, in described step 4, the aperture of mesoporous material is between 10-50nm.
Further improvement, in described step one, organic solvent is selected from toluene, acetone, ethyl acetate and ethanol; In described step 4, organic inert solvent is toluene or acetone.
Preparation method of the present invention is simple and reliable, and prepared modification electronic cigarette floccule has antibiotic property, not easily breed bacteria; Fiber surface is adsorbed with a large amount of mesoporous material simultaneously, has the attached performance of good adsorption/desorption to materials such as the nicotine in tobacco tar, solvent, essence and flavoring agents.Overcome electronic cigarette filler material over without antibiotic property, and the shortcoming of adsorption/desorption scarce capacity.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph on the dopamine modified fibre surface that embodiment 1 is prepared;
Fig. 2 is the stereoscan photograph on the mesoporous material modified fibre surface that embodiment 1 is prepared;
Fig. 3 is the stereoscan photograph on the mesoporous material modified fibre surface that embodiment 2 is prepared;
Fig. 4 is the stereoscan photograph on the mesoporous material modified fibre surface that embodiment 3 is prepared.
Detailed description of the invention
Embodiment 1
A preparation method for the cotton-shaped filler fiber of modification electronic cigarette, comprises the following steps:
Step one) electronic cigarette floccule is washed three times with toluene and acetone respectively, the floccule distilled water Ultrasonic Cleaning crossed with organic solvent washing 2 hours.
Step 2) 4-(2-amino-ethyl)-1,2-benzenediol is dissolved in distilled water, the concentration of this solution is 1mg/ml, then is 7 with trishydroxymethylaminomethane regulator solution pH.Take the cotton-shaped filler fiber 0.1g of washed electronic cigarette and add the 4-(2-amino-ethyl)-1 that 20ml prepares, in 2-resorcinol solution, react 24 hours under room temperature, the floccule distilled water of gained is washed, dry, obtain the cotton-shaped filler fiber of electronic cigarette (as shown in Figure 1) that adsorption has 4-(2-amino-ethyl)-1,2-benzenediol polymer.
Step 3) cotton-shaped for electronic cigarette filler fiber is joined in the toluene solution of 20ml toluene di-isocyanate(TDI), solution concentration is 5mg/ml, normal-temperature reaction 30 minutes.
Step 4) cotton-shaped for electronic cigarette filler fiber to be transferred in the toluene suspension of silicon-based mesoporous material, suspension concentration is 10mg/ml, normal-temperature reaction 30 minutes; Silicon-based mesoporous material is with poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) triblock copolymer for template, ethyl orthosilicate or for matrix obtain.Finally by fiber toluene, after ethanol washing, obtaining adsorption has the cotton-shaped filler fiber of the electronic cigarette of antiseptic and silicon-based mesoporous material.(as shown in Figure 2)
Embodiment 2
A preparation method for the cotton-shaped filler fiber of modification electronic cigarette, comprises the following steps:
Step one) electronic cigarette floccule is washed three times with ethyl acetate and ethanol respectively, cotton-shaped for the electronic cigarette crossed with organic solvent washing filler fiber distilled water Ultrasonic Cleaning 2 hours.
Step 2) by 3,4 dihydroxyphenylalanines are dissolved in distilled water, and the concentration of this solution is 5mg/ml, then is 8.5 with trishydroxymethylaminomethane regulator solution pH.Taking the cotton-shaped filler fiber 0.1g of washed electronic cigarette adds in 3, the 4 dihydroxyphenylalanine solution that 20ml prepares, and reacts 24 hours, is washed by cotton-shaped for the electronic cigarette of gained filler fiber distilled water, dry under room temperature.
Step 3) cotton-shaped for electronic cigarette filler fiber is joined in the toluene solution of 20ml bisphenol A type epoxy resin, solution concentration is 10mg/ml, normal-temperature reaction 30 minutes.
Step 4) will transfer in the toluene suspension of phenolic aldehyde based mesoporous material with electronic cigarette floccule, suspension concentration is 15mg/ml, adds potassium hydroxide as catalyst, and its consumption is 0.5%, 100 DEG C of reaction 4h; Phenolic aldehyde based mesoporous material take resol as matrix, and poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) triblock copolymer is obtained by template.Finally by gained floccule toluene, after ethanol washing, obtain the floccule that adsorption has antiseptic and phenolic aldehyde based mesoporous material.(as shown in Figure 3).
Embodiment 3
A preparation method for the cotton-shaped filler fiber of modification electronic cigarette, comprises the following steps:
Step one) electronic cigarette floccule is washed three times with ethanol and acetone respectively, the floccule distilled water Ultrasonic Cleaning crossed with organic solvent washing 2 hours.
Step 2) 3,4-dihydroxyphenyl-L-alanine of amino for the 4-of 3mg-1,2-catechol and 2mg is dissolved in 1000ml distilled water, then be 9 with trishydroxymethylaminomethane regulator solution pH.Take the cotton-shaped filler fiber 0.1g of washed electronic cigarette to add in amino-1, the 2-catechol of 4-and 4-dihydroxyphenylalanine mixed solution that 20ml prepares, react 24 hours under room temperature, the floccule distilled water of gained is washed, dry.
Step 3) cotton-shaped for electronic cigarette filler fiber is joined 4, in the toluene solution of 4 '-Biphenyl Ether dicarboxylic acid anhydride, solution concentration is 10mg/ml, normal-temperature reaction 30 minutes.
Step 4) the cotton-shaped filler fiber of electronic cigarette crossed with anhydride reaction to be transferred in the toluene suspension of silicon-based mesoporous material, suspension concentration is 15mg/ml, normal-temperature reaction 30 minutes; Silicon-based mesoporous material take amphipathic nature block polymer as template, and ethyl orthosilicate is that matrix obtains.Finally by fiber toluene, after ethanol washing, obtaining adsorption has the cotton-shaped filler fiber of the electronic cigarette of antiseptic and silicon-based mesoporous material.(as shown in Figure 4).
The properties of product of each embodiment as shown in Table 1 and Table 2, can be found out, compared with existing electronic cigarette filler, use the modified product of method of the present invention to have antibiotic property and better adsorption capacity.
Above example for illustration of the present invention, but is not used for limiting the scope of the invention, every following instance is done according to technical spirit of the present invention any simple modification, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
The each embodiment of table 1 prepares mesoporous material modified fibre surface adsorption property test result
The each embodiment of table 2 prepares mesoporous material modified fibre surface bacteriostasis property test result
Claims (12)
1. a preparation method for the cotton-shaped filler fiber of modification electronic cigarette, is characterised in that, comprises the following steps:
Step one: cotton-shaped filler fiber is first used organic solvent washing, then in water Ultrasonic Cleaning;
Step 2: cotton-shaped filler fiber is transferred in antimicrobial, takes out after complete reaction;
Step 3: cotton-shaped filler fiber is transferred in the solution containing difunctional coupling agent, takes out after complete reaction;
Step 4: cotton-shaped filler fiber and the mesoporous material containing active end group are reacted in organic inert solvent, obtains the cotton-shaped filler fiber of modification electronic cigarette with antibiotic property and high adsorption/desorption ability after complete reaction.
2. the preparation method of the cotton-shaped filler fiber of modification electronic cigarette as claimed in claim 1, it is characterized in that, in described step 2, antiseptic is organic phenolic antiseptic; Described organic phenolic antiseptic is any one or more than one mixing in 4-(2-amino-ethyl)-1,2-benzenediol, 3,4-dihydroxyphenyl-L-alanine, amino-1, the 2-catechol of 4-.
3. the preparation method of the cotton-shaped filler fiber of modification electronic cigarette as claimed in claim 2, it is characterized in that, the concentration of described organic phenolic antiseptic is 1-5mg/mL.
4. the preparation method of the cotton-shaped filler fiber of modification electronic cigarette as claimed in claim 1, it is characterized in that, in described step 2, the solvent of antimicrobial is water, adopts trishydroxymethylaminomethane to be that buffer regulates antimicrobial pH to 7-9.
5. the preparation method of the cotton-shaped filler fiber of modification electronic cigarette as claimed in claim 1, is characterized in that, in described step 3, difunctional coupling agent is any one in difunctional epoxy resin, difunctional isocyanates, difunctional acid anhydrides.
6. the preparation method of the cotton-shaped filler fiber of modification electronic cigarette as claimed in claim 5, it is characterized in that, the concentration of described difunctional coupling agent is 5-10mg/ml.
7. the preparation method of the cotton-shaped filler fiber of modification electronic cigarette as claimed in claim 1, it is characterized in that, in described step 4, mesoporous material is obtained by sol-gal process, and mesoporous material is carbon back mesoporous material or silicon-based mesoporous material.
8. the preparation method of the cotton-shaped filler fiber of modification electronic cigarette as claimed in claim 7, is characterized in that, in described step 4, carbon back mesoporous material take amphipathic nature block polymer as template, resol obtains for matrix; Silicon-based mesoporous material with amphipathic nature block polymer be template, ethyl orthosilicate for matrix obtain.
9. the preparation method of the cotton-shaped filler fiber of modification electronic cigarette as claimed in claim 7, it is characterized in that, in described step 4, silicon-based mesoporous material suspension concentration is 10-15mg/ml.
10. the preparation method of the cotton-shaped filler fiber of modification electronic cigarette as claimed in claim 1, it is characterized in that, in described step 4, the aperture of mesoporous material is between 10-50nm.
The preparation method of the cotton-shaped filler fiber of 11. modification electronic cigarette as claimed in claim 1, it is characterized in that, in described step one, organic solvent is selected from toluene, acetone, ethyl acetate and ethanol; In described step 4, organic inert solvent is toluene or acetone.
The preparation method of the cotton-shaped filler fiber of 12. modification electronic cigarette as claimed in claim 1, it is characterized in that, in described step one, organic solvent is selected from toluene, acetone, ethyl acetate and ethanol; In described step 4, organic inert solvent is toluene or acetone;
In described step 2, antiseptic is organic phenolic antiseptic; Described organic phenolic antiseptic is any one or more than one mixing in 4-(2-amino-ethyl)-1,2-benzenediol, 3,4-dihydroxyphenyl-L-alanine, amino-1, the 2-catechol of 4-; The concentration of described organic phenolic antiseptic is 1-5mg/mL; The solvent of antimicrobial is water, adopts trishydroxymethylaminomethane to be that buffer regulates antimicrobial pH to 7-9;
In described step 3, difunctional coupling agent is any one in difunctional epoxy resin, difunctional isocyanates, difunctional acid anhydrides; The concentration of described difunctional coupling agent is 5-10mg/ml;
In described step 4, mesoporous material is obtained by sol-gal process, and mesoporous material is carbon back mesoporous material or silicon-based mesoporous material; Carbon back mesoporous material with amphipathic nature block polymer be template, resol for matrix obtain; Silicon-based mesoporous material with amphipathic nature block polymer be template, ethyl orthosilicate for matrix obtain; Silicon-based mesoporous material suspension concentration is 10-15mg/ml; The aperture of mesoporous material is between 10-50nm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105504521A (en) * | 2016-01-29 | 2016-04-20 | 广西中烟工业有限责任公司 | Preparation method of electronic cigarette filter tip for capturing free radicals |
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| JP5460429B2 (en) * | 2010-04-02 | 2014-04-02 | 花王株式会社 | Textile treatment agent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105504521A (en) * | 2016-01-29 | 2016-04-20 | 广西中烟工业有限责任公司 | Preparation method of electronic cigarette filter tip for capturing free radicals |
| CN105504521B (en) * | 2016-01-29 | 2018-05-25 | 广西中烟工业有限责任公司 | A kind of preparation method for the electronics cigarette filter tip piece for capturing free radical |
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| CN105256536B (en) | 2017-12-19 |
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