CN110523352A - A kind of antibacterial phase-change microcapsule and preparation method thereof - Google Patents
A kind of antibacterial phase-change microcapsule and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of antibacterial phase-change microcapsules and preparation method thereof, comprising: restores silver in phase-change microcapsule surface in situ, prepares the antibacterial phase-change microcapsule with argentiferous;The present invention is silver-colored due to the lignin reduction for being surface of microcapsule, microcapsules contain a small amount of silver, it is at low cost, its high enthalpy for being not only able to maintain phase-change microcapsule, also there is excellent anti-microbial property, the method of the present invention has the features such as easy to operate, process flow is short, at low cost, has great application value in the fields such as daily textile and medical textile.
Description
Technical field
The invention belongs to antibacterial phase-change material and its preparation field, in particular to a kind of antibacterial phase-change microcapsule and its preparation
Method.
Background technique
Phase-change microcapsule is that phase-change material is wrapped in wall shell using microcapsules technology, forms small particle, thus
It prevents phase-change material from revealing, phase-change material is prevented to contact with the external world.Using the phase-change material of package phase is occurring for phase-change microcapsule
The characteristic for storing and releasing energy when transformation achievees the purpose that control material temperature, in food, weaving, medicine, coating, makeup
Product, transport, electronic device etc. are widely used.
Current its function of existing phase-change microcapsule is relatively single, is unable to satisfy that people are diversified to product function to be wanted
It asks, especially in daily textile or medical textile field, in constant same of the temperature for maintaining body temperature or use environment
When, bacterial growth or infection must be avoided as far as possible, this just proposes requirement to the antibiotic property of phase-change microcapsule.Chinese patent
CN106351017 provides a kind of microcapsules and preparation method thereof with mosquito repellent anti-bacterial heat storage temperature adjustment complex function, by phase transformation
The microcapsules that preparation has the temperature adjustment of mosquito repellent anti-bacterial heat storage are blended with the plants essential oil with mosquito repellent antibacterial functions for material, but it is used
Essential oil achievees the purpose that antibacterial, not persistently.Chinese patent CN108686262A provides a kind of sustained release based on double-walled microcapsules
The preparation method of antibacterial phase transformation medical dressing, using pretreated expanded perlite as carrier, after vacuum suction liquid state phase change material
In the chitosan layer of adsorption argentiferous, sodium alginate porous gel layer is re-formed, obtains double-walled sustained-release antibacterial phase-change microcapsule,
But it is porous material absorption phase-change material, and enthalpy is not high, and complex process.Chinese patent CN106351017A provides one
Kind has the microcapsules and preparation method thereof of mosquito repellent anti-bacterial heat storage temperature adjustment complex function, using composite core material (phase-change material and tool
Have the plants essential oil of mosquito repellent antibacterial) the mosquito repellent anti-bacterial heat storage temperature adjustment microcapsules using melamine resin as shell are prepared by in-situ polymerization,
But essential oil, which accounts for core material certain proportion, causes enthalpy not high, up to 81J/g.
Also there is the report of antibacterial phase-change microcapsule in pertinent literature.Geng et al (DOI:10.1016/
J.energy.2018.06.218 emulsifier) is made using styrene maleic anhydride copolymer and prepares phase-change microcapsule, is then deposited
Silver is deposited in surface of microcapsule, prepares silver-colored antibacterial phase-change microcapsule, enthalpy 170.2J/g.Wang et al (DOI:
It is 10.1016/j.energy.2018.06.118) that emulsified particle prepares the micro- glue of phase transformation using improved silica nanoparticle
Capsule, then using DEXTROSE ANHYDROUS as the reducing agent of silver ion in silica phase-change microcapsule surface reduction silver, preparation contains
Silver-colored antibacterial phase-change microcapsule, enthalpy 110.76J/g.But they use emulsifier and reducing agent substep preparation antibacterial phase transformation
Microcapsules cause preparation process cumbersome, complicated for operation, and microcapsules are both increased cost and also reduced by a large amount of silver coatings
Microcapsules enthalpy limits its industrial application.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of antibacterial phase-change microcapsules and preparation method thereof, overcome existing
Technology emulsifier and reducing agent substep preparation antibacterial phase-change microcapsule lead to the defect that technique is cumbersome, complicated for operation.Benefit of the invention
Use natural polymer lignin both as emulsifier and also make silver reducing agent, reduce the use of chemical reducing agent, easy to operate, work
Skill process is short;Moreover, the microcapsules of method preparation reduce cost containing a small amount of silver, moreover it is possible to guarantee the high enthalpy of microcapsules, assign
The good antibiotic property of microcapsules.
A kind of antibacterial phase-change microcapsule of the invention, which is characterized in that described for using the suspension of lignin phase-change microcapsule
The antibacterial phase-change microcapsule of area load silver is made in liquid and silver nitrate in situ.
A kind of preparation method of antibacterial phase-change microcapsule of the invention, comprising:
(1) using lignin suspension as water phase, and the phase-change material for containing isocyanate groups reagent is mixed as oily phase
It closes, emulsifying obtains emulsion oil-in-water;Then amine aqueous solution is added dropwise into emulsion oil-in-water, and stirs, obtains wood
Quality phase-change microcapsule suspension;
(2) silver nitrate solution will be added in above-mentioned lignin phase-change microcapsule suspension, stirs, filter, it is dry, resisted
Bacterium phase-change microcapsule.
The preferred embodiment of above-mentioned preparation method is as follows:
Lignin is the lignin particles of partial size 100-500nm in the step (1);Isocyanate groups reagent includes different
Isophorone diisocyanate IPDI, toluene di-isocyanate(TDI) TDI, methyl diphenylene diisocyanate MDI, two isocyanide of hexa-methylene
One or more of acid esters HDI;Phase-change material is long chain alkane phase-change material, general formula CnH2n+2, wherein n > 10;Amine examination
Agent includes ethylenediamine, hexamethylene diamine, triethylene diamine, one or more of four ethylene triamines, polyethyleneimine.
The mass fraction of lignin is 0.2-1.5% in lignin suspension in the step (1);Grease matter in lotion
Amount is than 1:9~1:1.It is 4000-15000rpm, homogenizing time that emulsifying, which is homogeneous revolution, in the step (1) are as follows: 1-
10min;Stirring rate is 100-1000rpm, time 1-8h.
The drop rate of amine aqueous solution is 1-10mL/min in the step (1).
The mass percentage concentration of silver nitrate solution is 1-10% in the step (2).
Filtering uses one of 500 mesh, 1000 mesh, 1200 mesh, the filter cloth of 1500 mesh in the step (2);Dry temperature
Degree is 30-120 DEG C, time 6-24h.
The present invention provides a kind of antibacterial phase-change microcapsule of the method preparation.
A kind of application of antibacterial phase-change microcapsule of the invention, such as daily textile and medical textile field.
Beneficial effect
There are the hydrophobic groupings such as hydrophilic radicals and phenyl ring such as hydroxyl in natural polymer lignin molecule structure, therefore have
Hydrophilic and hydrophobic can be used as the emulsified particle of pickering emulsion, meanwhile, hydroxyl or mercaptan on lignin can restore silver ion, wood
The shortcomings that quality also has inoxidizability, can inhibit argentiferous microcapsules silver is oxidized and reduces antibiotic property in use;
The present invention uses natural polymer lignin both as emulsifier or to make the reducing agent of silver, and one-step method prepares silver-containing antibacterial
Microcapsules, reduce the use of chemical reducing agent, easy to operate, process flow is short;Moreover, the microcapsules of method preparation are containing a small amount of
Silver reduces cost, moreover it is possible to guarantee the high enthalpy of microcapsules, assign the good antibiotic property of microcapsules, lignin also has anti-oxidant
Property, the shortcomings that capable of inhibiting argentiferous microcapsules silver is oxidized and reduces antibiotic property in use.
Detailed description of the invention
Argentiferous lignin phase-change microcapsule and lignin phase-change microcapsule SEM obtained in Fig. 1 embodiment 3 and comparative example 1
Figure;
The antibacterial test of argentiferous phase-change microcapsule obtained in Fig. 2 embodiment 3 and comparative example 1 (not argentiferous in comparative example 1)
Figure.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.Isocyanate reagents (MDI, TDI, IPDI etc.) purchase in embodiment is in Yantai Wanhua Polyurethane Company Limited public affairs
Department, amine reagent purchase are bought in Sinopharm Chemical Reagent Co., Ltd., lignin in the limited public affairs of Shandong Yang Hai environment-friendly materials
Department.
Embodiment 1
(1) the hexadecane paraffin that the fusing point of 1.8g is 18-20 DEG C is taken, the TDI (technical grade) of 0.2g is added thereto, then
Melt 10min at 30 DEG C, after mixing, the mass fraction for being added 30 DEG C of 18g temperature is that 0.4%, lignin partial size is about
The lignin suspension of 200nm, keeping temperature is 30 DEG C, emulsifying 3min, and homogeneous rate is 10000rpm, obtains hexadecane
Lotion.It takes 0.1g ethylenediamine reagent to be dissolved in 10g water, is preheating to 30 DEG C, then second is also gradually added dropwise in the hexadecane lotion in
Diamine solution, keep temperature be 30 DEG C, stirring rate 600rpm, stir 3h, obtain nucleocapsid than be about 9:1 phase-change microcapsule
Suspension.
(2) in Xiang Shangshu phase-change microcapsule suspension, the silver nitrate solution that 10g solubility is 1% is added, persistently stirs 8h,
Stirring rate is 300rpm, obtains the phase-change microcapsule suspension of argentiferous.
(3) it by the phase-change microcapsule suspension of the argentiferous in (2), with the filter-cloth filtering of 500 mesh, then dries at 30 DEG C
For 24 hours, dry powdered argentiferous phase-change microcapsule is obtained.
Embodiment 2
(1) the octadecane paraffin that the fusing point of 1.6g is 26-28 DEG C is taken, the MDI (technical grade) of 0.3g is added thereto, then
Melt 10min at 40 DEG C, after mixing, the mass fraction for being added 40 DEG C of 18g temperature is that 0.5%, lignin partial size is about
The lignin suspension of 300nm, keeping temperature is 40 DEG C, emulsifying 3min, and homogeneous rate is 8000rpm, obtains octadecane
Lotion.It takes 0.15g diethylenetriamine reagent to be dissolved in 10g water, is preheating to 40 DEG C, then the octadecane lotion in is also gradually dripped
Add diethylenetriamine solution, keeping temperature is 40 DEG C, stirring rate 800rpm, stirs 3h, obtain nucleocapsid than be about 4:1 phase
Become microcapsule suspensions.
(2) in Xiang Shangshu phase-change microcapsule suspension, the silver nitrate solution that 10g solubility is 2% is added, persistently stirs 8h,
Stirring rate is 300rpm, obtains the phase-change microcapsule suspension of argentiferous.
(3) it by the phase-change microcapsule suspension of the argentiferous in (2), with the filter-cloth filtering of 1000 mesh, then dries at 40 DEG C
20h obtains dry powdered argentiferous phase-change microcapsule.
Embodiment 3
(1) the eicosane paraffin that the fusing point of 1.5g is 35-37 DEG C is taken, the IPDI (technical grade) of 0.4g is added thereto, so
Melt 10min at 50 DEG C afterwards, after mixing, be added 18g temperature 50 C mass fraction be 0.6%, lignin partial size about
For the lignin suspension of 400nm, keeping temperature is 50 DEG C, emulsifying 3min, and homogeneous rate is 6000rpm, obtains 20
Alkane lotion.It takes 0.2g hexamethylene diamine to be dissolved in 10g water, is preheating to 50 DEG C, then oneself is also gradually added dropwise two in the eicosane lotion in
Amine aqueous solution, keep temperature be 50 DEG C, stirring rate 500rpm, stir 3h, obtain nucleocapsid than be about 2.5:1 phase-change microcapsule
Suspension.
(2) in Xiang Shangshu phase-change microcapsule suspension, the silver nitrate solution that 10g solubility is 1% is added, persistently stirs 8h,
Stirring rate is 300rpm, obtains the phase-change microcapsule suspension of argentiferous.
(3) it by the phase-change microcapsule suspension of the argentiferous in (2), with the filter-cloth filtering of 1200 mesh, then dries at 50 DEG C
16h obtains dry powdered argentiferous phase-change microcapsule.
There is complete spherical shape from the phase-change microcapsule that can see in comparative example 1 and embodiment 3 in the SEM figure in Fig. 1,
And lignin little particle on surface of microcapsule.It has also been found that argentiferous lignin phase-change microcapsule and lignin phase in amplified SEM
Change microcapsules are completely similar, will not be to lignin after illustrating the lignin little particle reduction silver ion on the shell of surface of microcapsule
Phase-change microcapsule generates the negative effect such as microcapsule aggregation, microcapsules broken shell.
From in Fig. 2 it can be found that the colony counts in the Escherichia coli of embodiment 3 and staphylococcus aureus culture dish are remote
Less than clump count in the culture dish of comparative example 1, illustrate that argentiferous phase-change microcapsule prepared by embodiment 3 is imitated with good antibacterial
Fruit.
Embodiment 4
(1) the docosane paraffin that the fusing point of 1.5g is 41-43 DEG C is taken, the HDI (technical grade) of 0.4g is added thereto, so
Melt 10min at 60 DEG C afterwards, after mixing, be added 18g temperature 60 C mass fraction be 0.6%, lignin partial size about
For the lignin suspension of 400nm, keeping temperature is 60 DEG C, emulsifying 3min, and homogeneous rate is 8000rpm, obtains 20
Dioxane lotion.It takes 0.1g hexamethylene diamine and 0.1g diethylenetriamine to be dissolved in 10g water, obtains mixing amine aqueous solution, be preheating to 60 DEG C, so
Mixing amine aqueous solution is also gradually added dropwise in docosane lotion in backward, and drop rate is that keeping temperature is 60 DEG C, and stirring rate is
500rpm, stir 3h, obtain nucleocapsid than be about 2.5:1 phase-change microcapsule suspension.
(2) in Xiang Shangshu phase-change microcapsule suspension, the silver nitrate solution that 10g solubility is 2% is added, persistently stirs 8h,
Stirring rate is 300rpm, obtains the phase-change microcapsule suspension of argentiferous.
(3) it by the phase-change microcapsule suspension of the argentiferous in (2), with the filter-cloth filtering of 1500 mesh, then dries at 60 DEG C
16h obtains dry powdered argentiferous phase-change microcapsule.
Comparative example 1
(1) the eicosane paraffin that the fusing point of 1.5g is 35-37 DEG C is taken, the IPDI (technical grade) of 0.4g is added thereto, so
Melt 10min at 50 DEG C afterwards, after mixing, be added 18g temperature 50 C mass fraction be 0.6%, lignin partial size about
For the lignin suspension of 400nm, keeping temperature is 50 DEG C, emulsifying 3min, and homogeneous rate is 6000rpm, obtains 20
Alkane lotion.It takes 0.2g hexamethylene diamine to be dissolved in 10g water, is preheating to 50 DEG C, then oneself is also gradually added dropwise two in the eicosane lotion in
Amine aqueous solution, keep temperature be 50 DEG C, stirring rate 500rpm, stir 3h, obtain nucleocapsid than be about 2.5:1 phase-change microcapsule
Suspension.
(2) in Xiang Shangshu phase-change microcapsule suspension, 10g water is added, persistently stirs 8h, stirring rate 300rpm is obtained
To phase-change microcapsule suspension.
(3) by the phase-change microcapsule suspension in (2), with the filter-cloth filtering of 1200 mesh, 16h then is dried at 50 DEG C, is obtained
To dry powdered phase-change microcapsule.
Statistics indicate that, compared with comparative example 1, argentiferous phase-change microcapsule argentiferous is prepared in embodiment 3 by Tables 1 and 2
Amount is not high, and enthalpy decline is less, still has preferable enthalpy 177J/g, has thermal storage and energy accumulation performance.Pass through the antibacterial in Fig. 2
Experiment also indicates that the argentiferous phase-change microcapsule in embodiment 3 also has good antibacterial effect.
Table 1: the tables of data of phase-change microcapsule obtained in embodiment 3 and comparative example 1
Sample | Enthalpy (J/g) | Surface silver content (%) |
N-eicosane | 257 | 0 |
Comparative example 1 | 179 | 0 |
Embodiment 3 | 177 | 2.32 |
Note: sample eicosane is the pure eicosane paraffin sample of the not microencapsulation in embodiment 3 and comparative example 1.
Table 2: the tables of data of antibacterial phase-change microcapsule compares in embodiment 3 and document/patent
Claims (10)
1. a kind of antibacterial phase-change microcapsule, which is characterized in that described for using lignin phase-change microcapsule suspension and silver nitrate
The antibacterial phase-change microcapsule of obtained area load silver in situ.
2. a kind of preparation method of antibacterial phase-change microcapsule, comprising:
(1) using lignin suspension as water phase, and the phase-change material for containing isocyanate groups reagent is mixed as oily phase,
Emulsifying obtains emulsion oil-in-water;Then amine aqueous solution is added dropwise into emulsion oil-in-water, and stirs,
Obtain lignin phase-change microcapsule suspension;
(2) silver nitrate solution will be added in above-mentioned lignin phase-change microcapsule suspension, stirs, filter, it is dry, obtain antibacterial phase
Become microcapsules.
3. preparation method according to claim 2, which is characterized in that lignin is partial size 100-500nm in the step (1)
Lignin particles;Isocyanate groups reagent includes isophorone diisocyanate IPDI, toluene di-isocyanate(TDI) TDI, and two
Methylenebis phenyl isocyanate MDI, one or more of hexamethylene diisocyanate HDI;Phase-change material is long chain alkane
Phase-change material, general formula CnH2n+2, wherein n > 10;Amine reagent includes ethylenediamine, hexamethylene diamine, triethylene diamine, four ethylene three
One or more of amine, polyethyleneimine.
4. preparation method according to claim 2, which is characterized in that lignin in lignin suspension in the step (1)
Mass fraction be 0.2-1.5%;Grease mass ratio 1:9~1:1 in lotion.
5. preparation method according to claim 2, which is characterized in that emulsifying is that homogeneous revolution is in the step (1)
4000-15000rpm, homogenizing time are as follows: 1-10min;Stirring rate is 100-1000rpm, time 1-8h.
6. preparation method according to claim 2, which is characterized in that the drop rate of amine aqueous solution in the step (1)
For 1-10mL/min.
7. preparation method according to claim 2, which is characterized in that the quality percentage of silver nitrate solution in the step (2)
Concentration is 1-10%.
8. preparation method according to claim 2, which is characterized in that in the step (2) filtering using 500 mesh, 1000 mesh,
One of 1200 mesh, filter cloth of 1500 mesh;Drying temperature is 30-120 DEG C, time 6-24h.
9. a kind of antibacterial phase-change microcapsule of claim 2 the method preparation.
10. the application of antibacterial phase-change microcapsule described in a kind of claim 1.
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CN112970749A (en) * | 2021-01-25 | 2021-06-18 | 湖北福力德鞋业有限责任公司 | Slow-release antibacterial microcapsule and preparation method thereof |
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