CN1795977A - Preparation method for loading functional in organic micromolecules - Google Patents
Preparation method for loading functional in organic micromolecules Download PDFInfo
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- CN1795977A CN1795977A CN 200410099225 CN200410099225A CN1795977A CN 1795977 A CN1795977 A CN 1795977A CN 200410099225 CN200410099225 CN 200410099225 CN 200410099225 A CN200410099225 A CN 200410099225A CN 1795977 A CN1795977 A CN 1795977A
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Abstract
The invention relates to a preparation method of nano hollow microsphere capable of loading functional organic small molecule. Said preparation method includes the step: in the presence of pressure difference loading the functional organic small molecule into the hollow cavity of nano hollow microsphere. The described functional organic small molecule can be existed in the solution or under the melting state. The invented nano hollow microsphere in which the functional organic small molecule is loaded can slowly release organic small molecule is loaded can slowly release organic antibacterial agent or organic antioxidant at the same time of having self-body inorganic antimicrobial property.
Description
Technical field
The present invention relates to the loading technique of a kind of functional organic molecule in the nano inorganic microballoon, relate in particular to the loading technique of functional organic molecule with antibiotic property and non-oxidizability.
Background technology
The technical research that has slow release effect in recent years is subjected to people's attention, the working time of proper extension functional component, when giving the new function of material, has saved cost.Have the carrier material of the hollow nano microballoon of core-shell type structure as a kind of novelty, the particularity of structure has determined it will have good application in the slowly-releasing field.
The preparation recent two decades of hollow nano microballoon has become the focus of domestic and international research, but the research of the application slowly-releasing in later stage is also relatively weak, and most of research concentrates on the medical science aspect, the for example loading of tumour medicine and slowly-releasing research, fixing and the releasing research of enzyme etc., the research aspect that is used as the macromolecular material auxiliary agent does not also see report.
Along with the fast development of macromolecular material, people expect more and more to give that macromolecular material is antibiotic, uvioresistant, anti-oxidant, even various functions such as antiviral.For example, the surface contamination of macromolecular material and bacteria breed bring threat for the people's health.People make in all sorts of ways to wait as hydrogen peroxide, alcohol, ozone, ultraviolet ray and suppress and killing bacteria.Yet these method timeliness are short, cost is high, not only uneconomical but also inconvenient.People wish to give macromolecular material these functions by adding functional aid.For example, by in macromolecular material, adding the anti-microbial property that antiseptic increases macromolecular material.Antiseptic mainly is divided into three kinds of natural class, mineral-type and organic classes.The natural antibacterial agent hear resistance is relatively poor, and range of application is narrower.That inorganic antiseptic has is long-acting, do not produce characteristics such as drug resistance, and outstanding hear resistance (＞600～1000) makes its application in materials such as plastics, chemical fibre, pottery in recent years enjoy attention.Organic antibacterial agent comprises multiple traditional antibiotic bactericide, sterilizing power is strong, effective, the source is abundant, but in its use, all exist service life short, hear resistance is relatively poor, easily run off in the processing, security is relatively poor, be easy to generate the microorganism drug resistance, easy deficiencies such as migration.Current, organic antibacterial agent is still antiseptic main product in the world, especially in American-European countries.As can be seen, the organic antibacterial agent of exploitation highly effective and safe, and be fixed in the macromolecule, the technology that plays a role for a long time by slowly-releasing has important market prospects.
Summary of the invention
Purpose of the present invention is exactly the preparation method that a kind of loading functional organic molecule hollow nano microballoon is provided for the defective that overcomes above-mentioned prior art existence.
Purpose of the present invention can be achieved through the following technical solutions: a kind of preparation method of loading functional organic molecule hollow nano microballoon, it is characterized in that, this preparation method is included under the situation that has pressure differential, functional organic molecule is loaded among the cavity of hollow nano microballoon, described functional organic molecule be in solution, exist or molten condition under exist.
Described preparation method specifically comprises the steps: the uniform hollow nano microballoon of particle diameter is placed container, and vacuum is taken out and pressed 20～40 minutes; Under atmospheric effect, certain density functional organic molecule solution is rushed in the container then; Under the condition of vacuum, stirred 24～48 hours; The functional organic molecule that centrifugal taking-up is unnecessary slowly is dried to Powdered.
Described hollow nano microballoon is a titania/inorganic carbon composite Nano hollow microsphere.
Described titania/inorganic carbon composite Nano hollow microsphere is to obtain by the template hydrolysis method.
The particle diameter of described hollow nano microballoon is 80～200nm.
Described functional organic molecule is the functional organic molecule with antibiotic, anti-oxidant or anti-ultraviolet function, comprises in alcohol system, phenol system, aldehyde system, organic acid system, ester system, ether system, peroxide epoxidation system, halogen system, imidazoles system, thiazole system, nitrile system, pyridine system, triazine system, quaternary ammonium salt system, organic metal system and the functional organic molecule of biguanides one or more.
Described functional organic molecule specifically is selected from isopropyl alcohol; 3 methyl 4 isopropyl phenol; formaldehyde; potassium sorbate; p-hydroxybenzoate; 2; 4; 4-three chloro-2 '-dihydroxy diphenyl ether is a triclosan; triumphant pine; imidazolidinyl urea; active climbazole; the trichlorine kappa; 3; 5 one dimethyl parachlorophenol Peracetic acid oxirane; N-(fluorine dichloromethyl sulphur) titanium acid imide; 2-(4-thiazolyl) benzimidazole (TBZ); 2-n-octyl-4-isothiazoline-3 ketone-; 2; 3; 5; the different peptide nitrile of 6-tetrachloro; the methylene cyanate ester; 2-pyridol-1-sodium oxide molybdena; N; N ' N "-the trihydroxy Hexahydrotriazine; benzyl dimethyl dodecyl chlorination ammonium is a benzalkonium bromide; copper 8-quinolinolate; 1, two [5-(4-chlorphenyl) biguanides] digluconate of 1-hexa-methylene; cycloalkyl hydroperoxide compound; salt anilid compound; the two phenoxy group arsenic of oxo; the benzophenone ethoxyquin; fourth hydroxyl methoxy benzene (BHA); in the Butylated Hydroxytoluene (BHT) one or more.
The solvent of the functional organic molecule of described dissolving is selected from one or more in ethanol, propyl alcohol, ethylene glycol, glycerine acetone, butanone, the ether.
The concentration of described functional organic molecule solution is 10～80% weight.
What the present invention made is a kind of slow release product, its release property testing process comprises the steps: that the hollow nano microballoon of getting the good functional organic molecule of quantitative loading is dissolved in the quantitative solvent, under condition of stirring, regularly accurately sampling, the functional organic molecule absorption intensity of ultra-violet analysis draws the release profiles of time and percentage by conversion.
The present invention has loaded the hollow nano microballoon of functional organic molecule, can slowly discharge organic antibacterial agent or organic oxidation-resistant agent when having inorganic antibacterial own, combines both advantages.
The present invention has loaded the hollow nano microballoon of functional organic molecule and can use in nylon, plastics, rubber, cosmetics, coating and medicine, obtains the function corresponding product.
Description of drawings
Fig. 1 is the TEM photo of titanium dioxide hollow microballoon of the present invention;
Fig. 2 has loaded the TEM photo of the titanium dioxide hollow microballoon of triclosan for the present invention;
Fig. 3 obtains the releasing curve diagram of product for the present invention.
The specific embodiment
Below in conjunction with drawings and the specific embodiments, the invention will be further described.
Embodiment 1
The hollow microsphere (see figure 1) of getting the 80-100nm of 0.05 gram places the boiling flask of 250ml, vacuum is taken out and was pressed 30 minutes, 20ml is contained 5 gram p-hydroxybenzoates, 2,4, the ethanolic solution of 4-three chloro-2 '-dihydroxy diphenyl ether (triclosan) is rushed in the boiling flask under atmospheric effect handle, under the situation of vacuum, stirs 48 hours, unnecessary triclosan is taken out in centrifugation, and slowly drying obtains loading triclosan hollow nano microballoon powder (see figure 2).Powder is dispersed in the 200ml ethanol, regularly accurately sampling, configuration ultraviolet specimen solution, data are analyzed in the ultraviolet test, obtain release profiles (curve 1 among Fig. 3).
Embodiment 2
The hollow microsphere of getting the 80-100nm of 0.05 gram places the boiling flask of 250ml, vacuum is taken out and was pressed 30 minutes, the ethanolic solution that 20ml is contained the 10 active climbazoles of gram (diazolones) is rushed in the boiling flask under atmospheric effect handle, under the situation of vacuum, stirred 48 hours, unnecessary active climbazole is taken out in centrifugation, and slowly drying obtains powder.Powder is dispersed in the 200ml ethanol, regularly accurately sampling, configuration ultraviolet specimen solution, data are analyzed in the ultraviolet test, obtain release profiles (curve 2 among Fig. 3).
Embodiment 3
The hollow microsphere of getting the 80-100nm of 0.05 gram places the boiling flask of 250ml, vacuum is taken out and was pressed 20 minutes, the acetone soln that 20ml is contained 5 gram triclosans is rushed in the boiling flask under atmospheric effect handle, under the situation of vacuum, stirred 48 hours, unnecessary triclosan is taken out in centrifugation, and slowly drying obtains powder.Powder is dispersed in the 200ml acetone, regularly accurately sampling, configuration ultraviolet specimen solution, data are analyzed in the ultraviolet test, obtain release profiles (curve 3 among Fig. 3).
Embodiment 4
The hollow microsphere of getting the 80-100nm of 0.05 gram places the boiling flask of 250ml, vacuum is taken out and was pressed 40 minutes, the ethanolic solution that 20ml is contained 2 gram benzophenone ethoxyquins is rushed in the boiling flask under atmospheric effect handle, under the situation of vacuum, stirred 24 hours, unnecessary benzophenone ethoxyquin is taken out in centrifugation, and slowly drying obtains powder.Powder is dispersed in the 200ml benzophenone, regularly accurately sampling, configuration ultraviolet specimen solution, data are analyzed in the ultraviolet test, obtain release profiles (curve 4 in the accompanying drawing 3).
Embodiment 5
The hollow microsphere of getting the 80-100nm of 0.05 gram places the boiling flask of 250ml, and 10 gram triclosans also are placed in one, and vacuum is taken out and pressed 30 minutes, boiling flask is placed on 80 ℃ of abundant middle heating of water, magnetic agitation 48 hours, unnecessary triclosan is taken out in centrifugation, and slowly drying obtains powder.Powder is dispersed in the 200ml ethanol, regularly accurately sampling, configuration ultraviolet specimen solution, data are analyzed in the ultraviolet test, obtain release profiles (curve 5 among Fig. 3).
Claims (9)
1. the preparation method of a loading functional organic molecule hollow nano microballoon, it is characterized in that, this preparation method is included under the situation that has pressure differential, functional organic molecule is loaded among the cavity of hollow nano microballoon, described functional organic molecule be in solution, exist or molten condition under exist.
2. the preparation method of a kind of loading functional organic molecule hollow nano microballoon according to claim 1, it is characterized in that, described preparation method specifically comprises the steps: the uniform hollow nano microballoon of particle diameter is placed container, and vacuum is taken out and pressed 20～40 minutes; Under atmospheric effect, certain density functional organic molecule solution is rushed in the container then; Under the condition of vacuum, stirred 24～48 hours; The functional organic molecule that centrifugal taking-up is unnecessary slowly is dried to Powdered.
3. the preparation method of a kind of loading functional organic molecule hollow nano microballoon according to claim 1 and 2 is characterized in that, described hollow nano microballoon is a titania/inorganic carbon composite Nano hollow microsphere.
4. the preparation method of a kind of loading functional organic molecule hollow nano microballoon according to claim 3 is characterized in that, described titania/inorganic carbon composite Nano hollow microsphere is to obtain by the template hydrolysis method.
5. the preparation method of a kind of loading functional organic molecule hollow nano microballoon according to claim 1 and 2 is characterized in that the particle diameter of described hollow nano microballoon is 80～200nm.
6. the preparation method of a kind of loading functional organic molecule hollow nano microballoon according to claim 1 and 2, it is characterized in that, described functional organic molecule is the functional organic molecule with antibiotic, anti-oxidant or anti-ultraviolet function, comprises in alcohol system, phenol system, aldehyde system, organic acid system, ester system, ether system, peroxide epoxidation system, halogen system, imidazoles system, thiazole system, nitrile system, pyridine system, triazine system, quaternary ammonium salt system, organic metal system and the functional organic molecule of biguanides one or more.
7. the preparation method of a kind of loading functional organic molecule hollow nano microballoon according to claim 6; it is characterized in that; described functional organic molecule specifically is selected from isopropyl alcohol; 3 methyl 4 isopropyl phenol; formaldehyde; potassium sorbate; p-hydroxybenzoate; 2; 4; 4-three chloro-2 '-dihydroxy diphenyl ether is a triclosan; triumphant pine; imidazolidinyl urea; active climbazole; the trichlorine kappa; 3; 5-dimethyl parachlorophenol Peracetic acid oxirane; N-(fluorine dichloromethyl sulphur) titanium acid imide; 2-(4-thiazolyl) benzimidazole (TBZ); 2-n-octyl-4-isothiazoline-3 ketone-; 2; 3; 5; the different peptide nitrile of 6-tetrachloro; the methylene cyanate ester; 2-pyridol-1-sodium oxide molybdena; N; N ' N "-the trihydroxy Hexahydrotriazine; benzyl dimethyl dodecyl chlorination ammonium is a benzalkonium bromide; copper 8-quinolinolate; 1, two [5-(4-chlorphenyl) biguanides] digluconate of 1-hexa-methylene; cycloalkyl hydroperoxide compound; salt anilid compound; the two phenoxy group arsenic of oxo; the benzophenone ethoxyquin; fourth hydroxyl methoxy benzene (BHA); in the Butylated Hydroxytoluene (BHT) one or more.
8. the preparation method of a kind of loading functional organic molecule hollow nano microballoon according to claim 1 and 2, it is characterized in that the solvent of the functional organic molecule of described dissolving is selected from one or more in ethanol, propyl alcohol, ethylene glycol, glycerine acetone, butanone, the ether.
9. the preparation method of a kind of loading functional organic molecule hollow nano microballoon according to claim 1 and 2 is characterized in that the concentration of described functional organic molecule solution is 10～80% weight.
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| CNB2004100992253A CN100528325C (en) | 2004-12-29 | 2004-12-29 | Preparation method for loading functional in organic micromolecules |
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| CN100528325C CN100528325C (en) | 2009-08-19 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921427A (en) * | 2010-08-06 | 2010-12-22 | 奇瑞汽车股份有限公司 | Functional high-polymer decorative composite material and preparation method thereof |
| CN101992049A (en) * | 2009-08-27 | 2011-03-30 | 华中科技大学 | Method for preparing porous nano-hollow sphere by self-assembled organic micromolecule acid-base double components |
| CN105542280A (en) * | 2016-01-20 | 2016-05-04 | 苏州市景荣科技有限公司 | Antibacterial deodorizing PE (polyethylene) sole material and preparation method thereof |
| CN106188644A (en) * | 2016-08-31 | 2016-12-07 | 河南恒发橡塑制品有限公司 | A kind of automobile interior exterior decorations environment-friendly antibacterial plastics and preparation method thereof |
| CN106380634A (en) * | 2016-08-31 | 2017-02-08 | 河南恒发橡塑制品有限公司 | Environmental-protection antibiosis sound-insulation plastic and production method thereof |
| CN107141474A (en) * | 2017-07-04 | 2017-09-08 | 南开大学 | It is poly- containing triclosan（β urethanes）Preparation method and the application in the streptococcus mutans biofilm of selectively killing oral cavity |
| CN108822378A (en) * | 2018-05-25 | 2018-11-16 | 湖北祥源新材科技股份有限公司 | Cross-linked foam polyolefin material and preparation method thereof with antibacterial functions |
| CN113493220A (en) * | 2020-04-02 | 2021-10-12 | 杨洋 | Hollow metal oxide microsphere, preparation method thereof and drug sustained-release application |
-
2004
- 2004-12-29 CN CNB2004100992253A patent/CN100528325C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101992049A (en) * | 2009-08-27 | 2011-03-30 | 华中科技大学 | Method for preparing porous nano-hollow sphere by self-assembled organic micromolecule acid-base double components |
| CN101992049B (en) * | 2009-08-27 | 2012-09-26 | 华中科技大学 | Method for preparing porous nano-hollow sphere by self-assembled organic micromolecule acid-base double components |
| CN101921427A (en) * | 2010-08-06 | 2010-12-22 | 奇瑞汽车股份有限公司 | Functional high-polymer decorative composite material and preparation method thereof |
| CN101921427B (en) * | 2010-08-06 | 2013-06-12 | 奇瑞汽车股份有限公司 | Functional high-polymer decorative composite material and preparation method thereof |
| CN105542280A (en) * | 2016-01-20 | 2016-05-04 | 苏州市景荣科技有限公司 | Antibacterial deodorizing PE (polyethylene) sole material and preparation method thereof |
| CN106188644A (en) * | 2016-08-31 | 2016-12-07 | 河南恒发橡塑制品有限公司 | A kind of automobile interior exterior decorations environment-friendly antibacterial plastics and preparation method thereof |
| CN106380634A (en) * | 2016-08-31 | 2017-02-08 | 河南恒发橡塑制品有限公司 | Environmental-protection antibiosis sound-insulation plastic and production method thereof |
| CN106188644B (en) * | 2016-08-31 | 2017-10-10 | 河南恒发橡塑制品有限公司 | A kind of automobile interior exterior decorations environment-friendly antibacterial plastics and preparation method thereof |
| CN106380634B (en) * | 2016-08-31 | 2017-10-10 | 河南恒发橡塑制品有限公司 | A kind of environment-friendly antibacterial sound insulation plastics and preparation method thereof |
| CN107141474A (en) * | 2017-07-04 | 2017-09-08 | 南开大学 | It is poly- containing triclosan（β urethanes）Preparation method and the application in the streptococcus mutans biofilm of selectively killing oral cavity |
| CN108822378A (en) * | 2018-05-25 | 2018-11-16 | 湖北祥源新材科技股份有限公司 | Cross-linked foam polyolefin material and preparation method thereof with antibacterial functions |
| CN113493220A (en) * | 2020-04-02 | 2021-10-12 | 杨洋 | Hollow metal oxide microsphere, preparation method thereof and drug sustained-release application |
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| Publication number | Publication date |
|---|---|
| CN100528325C (en) | 2009-08-19 |
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