CN110037017A - It is modified montmorillonite used and load plants essential oil antibacterial powder and preparation method thereof - Google Patents
It is modified montmorillonite used and load plants essential oil antibacterial powder and preparation method thereof Download PDFInfo
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- CN110037017A CN110037017A CN201910369656.3A CN201910369656A CN110037017A CN 110037017 A CN110037017 A CN 110037017A CN 201910369656 A CN201910369656 A CN 201910369656A CN 110037017 A CN110037017 A CN 110037017A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N31/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic oxygen or sulfur compounds
- A01N31/08—Oxygen or sulfur directly attached to an aromatic ring system
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N35/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical
- A01N35/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical containing aliphatically bound aldehyde or keto groups, or thio analogues thereof; Derivatives thereof, e.g. acetals
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Abstract
Montmorillonite is added in distilled water and is dispersed with stirring by the present invention, adds cetyl trimethylammonium bromide water-bath oscillation, is washed with distilled water and dries after filtering, grinds and obtain smectite powder.Smectite powder is added in 50% ethyl alcohol and is dispersed, plants essential oil water-bath oscillation is then added, obtains modified montmorillonite used with 50% ethanol washing and drying, grinding after filtering and loads plants essential oil antibacterial powder.Plants essential oil is loaded on montmorillonite, its stability can be improved, prepares the organic/inorganic type composite antibacterial material for having both absorption and anti-microbial property.The present invention selects montmorillonite as carrier, and cheap and easy to get, using antibacterial powder prepared by the plants essential oil in modified montmorillonite adsorbent solution, not only industrial cost is lower, but also process flow is simplified and nontoxic.In addition, montmorillonite passes through modified back loading plants essential oil in the present invention, the load factor of plants essential oil is improved, and have good fungistatic effect to staphylococcus aureus and Escherichia coli.
Description
Technical field:
The present invention relates to anti-biotic material preparation technical fields, specifically, being related to a kind of modified montmorillonite used and loading plant
Essential oil antibacterial powder and preparation method thereof.
Background technique:
Germ contamination is always the problem that a comparison is serious in the industries such as food, packaging, cosmetics, medical treatment, health care.It is anti-
Raw element once had good inhibiting effect to germ contamination, but due to being used for a long time, bacterium gradually produces drug resistance, can only be by increasing
Add dosage, this causes environmental pollution again.Therefore, the research and development and application of novel antibacterial material have become pre- preventing microbial contamination
The hot issue of generation.For this purpose, various anti-biotic materials have been extensively studied in people, such as utilize silver, copper, zinc, titanium, mercury, lead metal
And its inorganic antibacterial material made from ion, quaternary ammonium salt, biguanides, alcohols, phenols, organic amine, pyridines etc. are organic anti-
The natural antibacterial materials such as bacterium material and terpene, alkaloid, flavones, steroidal.
Inorganic anti-biotic material heat resisting temperature is higher, long service life, but the occasion and condition that use have considerable restraint；
Organic anti-biotic material sterilization speed is fast, and anti-microbial property is good, but its heat resistance is poor, easy to migrate, easily causes secondary pollution；It
Right class anti-biotic material natural environmental-protective, nontoxic, good biocompatibility, but extract processing difficulties, poor heat resistance, broad-spectrum long-acting
Property is weaker.All kinds of single anti-biotic materials have its advantage and disadvantage and more suitable field.
A large amount of result of study shows that some natural plant essential oils have certain antiseptic and inhibiting bacteria function effect, in fragrant plant
The antipathogenic composition being rich in increasingly is taken seriously, and becomes the popular materials of exploitation new type natural anti-biotic material.Common natural plant
Effective antimicrobial component has carvacrol, Thymol, cinnamic acid etc. in object essential oil.Antibacterial plant essential oil has good and safe antibacterial
Performance, but its is volatile, stability is poor, this is applied to produce certain limitation.
In the prior art, essential oil is fixed has in the method for improving its stability and antibiotic property:
One is microcapsules are made in essential oil embedding.Emulsifier is added in essential oil and carries out emulsifying formation capsule-core solution,
Capsule-core solution is mixed with capsule wall solution, homogeneous obtains emulsion, using spray drying or vacuum freeze drying to emulsion into
Row is dried to obtain microcapsules.
Another kind is that inclusion compound is made in essential oil embedding.Beta-cyclodextrin saturated aqueous solution is prepared first, then presses essential oil
It is added to preparation essential oil solution in solvent according to certain volume ratio, is instilled according to a certain percentage into beta-cyclodextrin saturated aqueous solution
Mountain essential oil solution stirs, and stands, and makes Precipitation, and precipitating is collected in filtering, and washing, freeze-drying obtain essential oil clathrate.
There are also one is essential oil is fixed on carrier.Essential oil and macromolecule carrier mixing first, by mixture in ball milling
Ball milling obtains essential oil solid dispersions in machine.
The above method not can solve the problem that natural plant essential oils are volatile, stability is poor.And it uses suitable
When carrier material the composite antibacterial material better than single anti-biotic material can be prepared using inorganic/organic complex method
Material.
Summary of the invention:
An object of the present invention is using inorganic/organic complex method, and it is good, not volatile to provide a kind of stability,
It has both the modified montmorillonite used of absorption and anti-microbial property and loads plants essential oil antibacterial powder.
The second object of the present invention is to provide a kind of preparation method that is modified montmorillonite used and loading plants essential oil antibacterial powder.
One kind is modified montmorillonite used and loads plants essential oil antibacterial powder, which is characterized in that including following parts by weight of component: modified
1 part of montmorillonite powder, 0.5~1 part of plants essential oil, the plants essential oil is carried on modified montmorillonite used.
Preferably, the smectite powder is dispersed with stirring by the way that montmorillonite original powder to be added in distilled water, adds ten
Six alkyl trimethyl ammonium bromide water-baths oscillation, then be centrifuged or filtered separation, washing, drying, grinding obtain.
Preferably, the plants essential oil is one or more of carvacrol, Thymol and cinnamic acid.
Preparation method that is a kind of modified montmorillonite used as described in claim 1 and loading plants essential oil antibacterial powder, including it is following
Step:
(1) it prepares modified montmorillonite used: montmorillonite original powder being added in appropriate distilled water and is dispersed with stirring, add montmorillonite sun
3~12h, centrifugation are vibrated in the cetyl trimethylammonium bromide that 0.75~1.5 times of ion exchange capacity, 40~80 DEG C of condition water-baths
Or separation solid liquid phase is filtered, and solid phase is washed with distilled water 3~5 times, then dry at 40~80 DEG C, grinding is modified
Montmorillonite powder；
(2) it loads plants essential oil: smectite powder obtained by step (1) being added in 50% ethanol solution and is stirred, is obtained
Modified montmorillonite used dispersion liquid, then be in mass ratio load plants essential oil: modified montmorillonite used=1:(1~2) addition plants essential oil, 40
~60 DEG C of condition water-bath oscillations 12~for 24 hours, centrifugation or suction filtration separation solid liquid phase, and solid phase is washed 3~5 with 50% ethanol solution
Time, it is then dry at 40~60 DEG C, it grinds to obtain the final product modified montmorillonite used and loads plants essential oil antibacterial powder.
Preferably, the plants essential oil is one or more of carvacrol, Thymol and cinnamic acid.
Preferably, the montmorillonite original powder purity in the step (1) is >=95%.
Preferably, the montmorillonite original powder cation exchange capacity in the step (1) is 80~150mmol/100g.
Preferably, the amount of cetyl trimethylammonium bromide is the 1 of montmorillonite cation exchange capacity in the step (1)
Times, water-bath vibration temperature is 60 DEG C, time 6h, and drying temperature is 60 DEG C.
Preferably, plants essential oil and modified montmorillonite used mass ratio are 1:1.5 in the step (2), and water-bath vibration temperature is
50 DEG C, time 18h, drying temperature is 50 DEG C.
Preferably, step (1) grind size is 200~300 mesh, and step (2) grind size is 200~300
Mesh.
Montmorillonite is added in distilled water and is dispersed with stirring by the present invention, adds cetyl trimethylammonium bromide water-bath vibration
It swings, is washed with distilled water and dries after filtering, grinding obtains smectite powder.Smectite powder is added in 50% ethyl alcohol
Dispersion, then be added plants essential oil water-bath oscillation, after filtering with 50% ethanol washing and drying, grinding obtain it is modified montmorillonite used simultaneously
Load plants essential oil antibacterial powder.Plants essential oil is loaded on montmorillonite, its stability can be improved, is prepared and is had both absorption and resist
The organic/inorganic type composite antibacterial material of bacterium performance.
The present invention selects montmorillonite as carrier, cheap and easy to get, utilizes the plant in modified montmorillonite adsorbent solution
Not only industrial cost is lower for antibacterial powder prepared by essential oil, but also process flow is simplified and nontoxic.In addition, being covered in the present invention
De- stone passes through modified back loading plants essential oil, improves the load factor of plants essential oil, and to staphylococcus aureus and large intestine
Bacillus has good fungistatic effect.
Detailed description of the invention
Fig. 1 is the XRD spectra of MMT, CTAB/MMT, Car-CTAB/MMT and Thy-CTAB/MMT；
Fig. 2 is the infrared spectrogram of Carvaceol, CTAB/MMT and Car-CTAB/MMT；
Fig. 3 is the infrared spectrogram of Thymol, CTAB/MMT and Thy-CTAB/MMT；
Fig. 4 is the thermogravimetric curve of MMT, CTAB/MMT and Car-CTAB/MMT；
Fig. 5 is the thermogravimetric curve of MMT, CTAB/MMT and Thy-CTAB/MMT.
Specific embodiment:
Embodiment 1:
(1) prepare modified montmorillonite used: choosing purity as >=95%, cation exchange capacity is 80~100mmol/100g's
Montmorillonite original powder is added in appropriate distilled water and is dispersed with stirring, adds montmorillonite cation exchange capacity 0.8 by montmorillonite original powder
3h are vibrated in cetyl trimethylammonium bromide again, 80 DEG C of condition water-baths, are centrifugated solid liquid phase, and solid phase distillation is washed
It washs 3 times, it is then dry at 50 DEG C, it is ground to 200~250 mesh and obtains smectite powder；
(2) preparation carries carvacrol antibacterial powder: taking dehydrated alcohol and distilled water, 1:1 obtains 50% ethyl alcohol by volume, will walk
Suddenly smectite powder obtained by (1) is added in 50% ethanol solution and stirs, and water-bath is carried out at 60 DEG C and vibrates 1h, obtains modified illiteracy
De- stone dispersion liquid, then be in mass ratio carvacrol: carvacrol is added in modified montmorillonite used=1:1, continues water-bath and vibrates 12h, centrifugation
Solid liquid phase is separated, and solid phase is washed 3 times with 50% ethanol solution, it is then dry at 55 DEG C, it is ground to 250~300 mesh i.e.
It obtains modified montmorillonite used and loads carvacrol antibacterial powder sample I.The adsorbance of carvacrol is in unmodified montmorillonite antibacterial powder
8.24wt%, and the adsorbance of carvacrol is 13.42wt% in modified montmorillonite used antibacterial powder.
(3) carvacrol (13.42wt%) antibacterial powder and montmorillonite original powder are carried made of determination step (2) to golden yellow grape
The minimal inhibitory concentration and minimum bactericidal concentration of coccus and Escherichia coli.After measured, montmorillonite original powder does not have antibacterial activity；Sheep's-parsley
Phenol is respectively 125 μ g/mL and 250 μ g/mL to the minimal inhibitory concentration and minimum bactericidal concentration of staphylococcus aureus, carries Sheep's-parsley
Phenol antibacterial powder is respectively 58 μ g/mL and 233 μ g/mL to the minimal inhibitory concentration and minimum bactericidal concentration of staphylococcus aureus,
Wherein the concentration of carvacrol is respectively 8 μ g/mL and 31 μ g/mL；Carvacrol kills the minimal inhibitory concentration and minimum of Escherichia coli
Bacteria concentration is respectively 125 μ g/mL and 250 μ g/mL, carries carvacrol antibacterial powder and kills to the minimal inhibitory concentration and minimum of Escherichia coli
Bacteria concentration is respectively 466 μ g/mL and 931 μ g/mL, and wherein the concentration of carvacrol is respectively 63 μ g/mL and 125 μ g/mL.
Embodiment 2:
(1) prepare modified montmorillonite used: choosing purity is that the illiteracy that >=97%, cation exchange capacity is 120mmol/100g is de-
Montmorillonite original powder is added in appropriate distilled water and is dispersed with stirring, adds the ten of 1 times of montmorillonite cation exchange capacity by stone original powder
Six alkyl trimethyl ammonium bromides, 40 DEG C of condition water-baths vibrate 9h, are centrifugated solid liquid phase, and solid phase is washed with distilled water 3 times,
Then dry at 40 DEG C, it is ground to 250 mesh and obtains smectite powder；
(2) preparation carries Thymol antibacterial powder: taking dehydrated alcohol and distilled water, 1:1 obtains 50% ethyl alcohol by volume, will
Smectite powder obtained by step (1) is added in 50% ethanol solution and stirs, and water-bath is carried out at 40 DEG C and vibrates 1h, is modified
Montmorillonite dispersion liquid, then be in mass ratio Thymol: Thymol is added in modified montmorillonite used=1:1.7, continues water-bath oscillation
16h is centrifugated solid liquid phase, and solid phase is washed 3 times with 50% ethanol solution, then dries at 60 DEG C, it is ground to 250~
300 mesh are up to modified montmorillonite used and load Thymol antibacterial powder sample II.Thymol in unmodified montmorillonite antibacterial powder
Adsorbance is 4.51wt%, and the adsorbance of Thymol is 10.05wt% in modified montmorillonite used antibacterial powder.
(3) Thymol (10.05wt%) antibacterial powder and montmorillonite original powder are carried made of determination step (2) to golden yellow Portugal
The minimal inhibitory concentration and minimum bactericidal concentration of grape coccus and Escherichia coli.After measured, montmorillonite original powder does not have antibacterial activity；Hundred
In fragrant phenol be respectively 125 μ g/mL and 250 μ g/mL to the minimal inhibitory concentration and minimum bactericidal concentration of staphylococcus aureus, carry
Thymol antibacterial powder is respectively 78 μ g/mL and 311 μ to the minimal inhibitory concentration and minimum bactericidal concentration of staphylococcus aureus
G/mL, wherein the concentration of Thymol is respectively 8 μ g/mL and 31 μ g/mL；Minimal inhibitory concentration of the Thymol to Escherichia coli
It is respectively 125 μ g/mL and 250 μ g/mL with minimum bactericidal concentration, it is antibacterial dense to the minimum of Escherichia coli carries Thymol antibacterial powder
Degree and minimum bactericidal concentration are respectively 622 μ g/mL and 1244 μ g/mL, wherein the concentration of Thymol be respectively 63 μ g/mL and
125μg/mL。
Embodiment 3:
(1) prepare modified montmorillonite used: choosing purity as >=99%, cation exchange capacity is 130~150mmol/100g
Montmorillonite original powder, montmorillonite original powder is added in appropriate distilled water and is dispersed with stirring, montmorillonite cation exchange capacity is added
6h is vibrated in 1.2 times of cetyl trimethylammonium bromide, 60 DEG C of condition water-baths, is centrifugated solid liquid phase, and solid phase is distilled
It is water washing 3 times, then dry at 80 DEG C, it is ground to 250~300 mesh and obtains smectite powder；
(2) preparation carries cinnamic acid antibacterial powder: taking dehydrated alcohol and distilled water, 1:1 obtains 50% ethyl alcohol by volume, will walk
Suddenly smectite powder obtained by (1) is added in 50% ethanol solution and stirs, and water-bath is carried out at 50 DEG C and vibrates 1h, obtains modified illiteracy
De- stone dispersion liquid, then be in mass ratio cinnamic acid: cinnamic acid is added in modified montmorillonite used=1:2, continues water-bath and vibrates 20h, centrifugation
Solid liquid phase is separated, and solid phase is washed 3 times with 50% ethanol solution, it is then dry at 50 DEG C, it is ground to 200~250 mesh i.e.
It obtains modified montmorillonite used and loads cinnamic acid antibacterial powder sample III.The adsorbance of cinnamic acid is in unmodified montmorillonite antibacterial powder
6.31wt%, and the adsorbance of cinnamic acid is 10.37wt% in modified montmorillonite used antibacterial powder.
(3) cinnamic acid (10.37wt%) antibacterial powder is carried made of standard broth Dilution step (2) and montmorillonite is former
Minimal inhibitory concentration and minimum bactericidal concentration of the powder to staphylococcus aureus and Escherichia coli.After measured, montmorillonite original powder does not have
There is antibacterial activity；Cinnamic acid to the minimal inhibitory concentration and minimum bactericidal concentration of staphylococcus aureus be respectively 250 μ g/mL and
500 μ g/mL, carrying cinnamic acid antibacterial powder is respectively 151 μ to the minimal inhibitory concentration and minimum bactericidal concentration of staphylococcus aureus
G/mL and 603 μ g/mL, wherein the concentration of cinnamic acid is respectively 16 μ g/mL and 63 μ g/mL；Minimum of the cinnamic acid to Escherichia coli
Mlc and minimum bactericidal concentration are respectively 250 μ g/mL and 500 μ g/mL, carry cinnamic acid antibacterial powder to the minimum of Escherichia coli
Mlc and minimum bactericidal concentration are respectively 1205 μ g/mL and 4820 μ g/mL, and wherein the concentration of cinnamic acid is respectively 125 μ g/
ML and 500 μ g/mL.
Embodiment 4:
(1) prepare modified montmorillonite used: choosing purity is that the illiteracy that >=98%, cation exchange capacity is 140mmol/100g is de-
Montmorillonite original powder is added in appropriate distilled water and is dispersed with stirring, adds 1.5 times of montmorillonite cation exchange capacity by stone original powder
Cetyl trimethylammonium bromide, 80 DEG C of condition water-baths vibrate 3h, are centrifugated solid liquid phase, and solid phase is washed with distilled water 3
Time, it is then dry at 60 DEG C, it is ground to 250 mesh and obtains smectite powder；
(2) preparation carries carvacrol antibacterial powder: taking dehydrated alcohol and distilled water, 1:1 obtains 50% ethyl alcohol by volume, will walk
Suddenly smectite powder obtained by (1) is added in 50% ethanol solution and stirs, and water-bath is carried out at 60 DEG C and vibrates 1h, obtains modified illiteracy
De- stone dispersion liquid, then be in mass ratio carvacrol: carvacrol is added in modified montmorillonite used=1:1.5, continues water-bath oscillation for 24 hours, from
The heart separates solid liquid phase, and solid phase is washed 3 times with 50% ethanol solution, then dry at 40 DEG C, is ground to 300 mesh and changes to obtain the final product
Property montmorillonite simultaneously loads carvacrol antibacterial powder sample IV.The adsorbance of carvacrol is in unmodified montmorillonite antibacterial powder
8.24wt%, and the adsorbance of carvacrol is 15.79wt% in modified montmorillonite used antibacterial powder.
(3) carvacrol (15.79wt%) antibacterial powder and montmorillonite original powder are carried made of determination step (2) to golden yellow grape
The minimal inhibitory concentration and minimum bactericidal concentration of coccus and Escherichia coli.After measured, montmorillonite original powder does not have antibacterial activity；Sheep's-parsley
Phenol is respectively 125 μ g/mL and 250 μ g/mL to the minimal inhibitory concentration and minimum bactericidal concentration of staphylococcus aureus, carries Sheep's-parsley
Phenol antibacterial powder is respectively 49 μ g/mL and 198 μ g/mL to the minimal inhibitory concentration and minimum bactericidal concentration of staphylococcus aureus,
Wherein the concentration of carvacrol is respectively 8 μ g/mL and 31 μ g/mL；Carvacrol kills the minimal inhibitory concentration and minimum of Escherichia coli
Bacteria concentration is respectively 125 μ g/mL and 250 μ g/mL, carries carvacrol antibacterial powder and kills to the minimal inhibitory concentration and minimum of Escherichia coli
Bacteria concentration is respectively 198 μ g/mL and 792 μ g/mL, and wherein the concentration of carvacrol is respectively 31 μ g/mL and 125 μ g/mL.
Essential oil load capacity before and after 1 cetyl trimethylammonium bromide Modification of Montmorillonite of table
Minimal inhibitory concentration and minimum bactericidal concentration of 2 material of table to Escherichia coli
Minimal inhibitory concentration and minimum bactericidal concentration of 3 material of table to staphylococcus aureus
It can be seen that by the data of table 1 to table 3 according to the modified montmorillonite used of this method preparation and load plants essential oil,
Plants essential oil is carried on modified montmorillonite used, essential oil load capacity is significantly increased relative to unmodified montmorillonite, increases plant essence
The stability of oil, wherein the adsorbance of carvacrol is in the modified montmorillonite used antibacterial powder of sample IV prepared by specific embodiment 4
15.79wt%.At the same time, this method preparation it is modified montmorillonite used and load plants essential oil, increasing the steady of plants essential oil
On the basis of qualitatively, there are good fungistatic effect and bactericidal effect to staphylococcus aureus and Escherichia coli.It is measured, is had
Sample IV prepared by body embodiment 4, the 198 μ g/mL that can reach minimum to the minimal inhibitory concentration of Escherichia coli (it is anti-to carry Thymol
Bacterium powder, 31 μ g/mL of Sheep's-parsley phenol content), the minimum 792 μ g/mL that can reach of minimum bactericidal concentration (carry Thymol antibacterial powder, Sheep's-parsley
125 μ g/mL of phenol content)；Can reach 49 μ g/mLs minimum to the minimal inhibitory concentration of staphylococcus aureus (it is anti-to carry Thymol
Bacterium powder, 8 μ g/mL of Sheep's-parsley phenol content), the minimum 198 μ g/mL that can reach of minimum bactericidal concentration (carry Thymol antibacterial powder, carvacrol
31 μ g/mL of content).
X-ray diffraction analysis:
X-ray diffraction method is the detection common method of intercalation effect.It is weak from peak position out and peak intensity, it can detecte out
The effect of montmorillonite layer spacing size and intercalation.It is calculated using the position that montmorillonite characteristic diffraction peak occurs by Bragg equation
Corresponding interlamellar spacing can verify that whether antibacterial agent enters the interlayer of montmorillonite by the variation of interlamellar spacing.Fig. 1 is MMT (montmorillonite
Original powder), CTAB/MMT (cetyl trimethylammonium bromide smectite powder), Car-CTAB/MMT (sample in specific embodiment 1
Product I) and Thy-CTAB/MMT (sample II in specific embodiment 2) XRD spectrum.From figure 1 it appears that MMT is equal in 2 θ
The strong diffraction maximum occurred at 5.79 ° corresponds to the bottom reflection in montmorillonite (001) face, CTAB/MMT, Car-CTAB/MMT and
There is strong diffraction maximum at 4.27 °, 3.79 ° and 3.42 ° respectively in Thy-CTAB/MMT, and the bottom surface in corresponding montmorillonite (001) face is anti-
It penetrates.Interlamellar spacing is increased to 2.07nm, 2.33nm and 2.58nm by the 1.52nm of sodium-based montmorillonite respectively, illustrates cetyl front three
Base ammonium bromide, carvacrol and Thymol enter between montmorillonite layer, change the interlayer structure of montmorillonite, montmorillonite layer spacing
Become larger.After the modified montmorillonite-loaded carvacrol of cetyl trimethylammonium bromide and Thymol its interlamellar spacing variation compared with
It is small, it may be possible to which that the carvacrol and Thymol majority of load are adsorbed on montmorillonite surface and only fraction enters the knot of interlayer
Fruit.
Infrared spectrum analysis:
Fig. 2 be Carvaceol (carvacrol), CTAB/MMT (cetyl trimethylammonium bromide smectite powder) and
The infrared spectrogram of Car-CTAB/MMT (sample I in specific embodiment 1), from Figure 2 it can be seen that before load carvacrol and Thymol
The infrared spectroscopy peak shape of CTAB/MMT is almost the same afterwards, the characteristic absorption peak of montmorillonite: 3624.55cm occurs-1The suction at place
Receiving peak is hydroxyl stretching vibration absworption peak in Al-O-H, 1031.99cm-1Place is that octahedron Si-O-Si stretches in montmorillonite lattice
Contracting vibration absorption peak, 800-400cm-1Place is the bending vibration absorption peak of Al-O and Si-O, 3430.41cm-1And 1642.79cm-1
The absorption peak at place is respectively the stretching vibration absworption peak and bending vibration absorption peak of layer structural water hydroxyl O-H.2925.41cm-1
And 2853.19cm-1The absorption peak at place is due to CH in CTAB2And CH3The stretching vibration of group.It can be seen by comparing spectral line
Out, it is compared with CTAB/MMT, following variation: 3019.14cm has occurred in Car-CTAB/MMT infrared spectrogram-1There is phenyl ring in place
The stretching vibration absworption peak of C-H；1591.05cm-1、1514.39cm-1、1418.93cm-1Place is that the carbon skeleton of phenyl ring vibrates；
1381.03cm-1There is CH in place3Flexural vibrations peak.
Fig. 3 be Thymol (Thymol), CTAB/MMT (cetyl trimethylammonium bromide smectite powder) and
The infrared spectrogram of Thy-CTAB/MMT (sample II in specific embodiment 2) compares, Thy- as seen from Figure 3 with CTAB/MMT
The Main change that CTAB/MMT infrared spectrogram occurs are as follows: 3024.45cm-1There is the stretching vibration absworption peak of phenyl ring C-H in place；
1617.48cm-1、1584.30cm-1、1419.85cm-1It is vibrated for the carbon skeleton of phenyl ring；1380.84cm-1There is CH in place3It is curved
Bent vibration peak.Show that carvacrol and Thymol have loaded on carrier structure in conjunction with XRD conclusion.
Thermogravimetic analysis (TGA):
Figure 4 and 5 are Car-CTAB/MMT (sample I in specific embodiment 1) and Thy-CTAB/MMT (specific embodiment respectively
Sample II in 2) thermogravimetric curve.As seen from the figure, Car-CTAB/MMT and Thy-CTAB/MMT thermogravimetric curve can be divided into four
Stage: accounting for about the 1.65% and 2.41% of two kinds of composite material gross masses in 30~100 DEG C of weightlessness, is due to adsorbing water
Caused by desorption, constant weight is kept later；It in 150~250 DEG C of weightlessness is made by the thermal decomposition of carvacrol and Thymol
At, 8.48% and 9.56% or so of gross mass, shows that carvacrol and Thymol successfully load on CTAB/MMT respectively；
Weight-loss ratio between 250~500 DEG C accounts for 22.15% and 23.1% or so respectively, is as caused by the thermal decomposition of CTAB molecule；500
~800 DEG C of weightlessness is then as caused by the structure dehydroxylation of montmorillonite mineral, and weight-loss ratio accounts for 2.94% He of gross mass respectively
3.12% or so.Between 30~100 DEG C, the mass loss ratio of CTAB/MMT, Car-CTAB/MMT and Thy-CTAB/MMT
Significantly lower than MMT, illustrate montmorillonite through cetyl trimethylammonium bromide it is organically-modified after, surface adsorption water is reduced.250
Main frame is stablized before DEG C, shows that the material base has preferable stability.
Claims (10)
1. one kind is modified montmorillonite used and loads plants essential oil antibacterial powder, which is characterized in that including following parts by weight of component: modified to cover
De- 1 part of mountain flour, 0.5~1 part of plants essential oil, the plants essential oil is carried on modified montmorillonite used.
2. as described in claim 1 modified montmorillonite used and load plants essential oil antibacterial powder, which is characterized in that it is described it is modified cover it is de-
Mountain flour is dispersed with stirring by the way that montmorillonite original powder to be added in distilled water, adds cetyl trimethylammonium bromide water-bath oscillation,
It is centrifuged or is filtered again separation, washing, drying, grinding obtain.
3. as described in claim 1 modified montmorillonite used and load plants essential oil antibacterial powder, which is characterized in that the plants essential oil
For one or more of carvacrol, Thymol and cinnamic acid.
4. preparation method that is a kind of modified montmorillonite used as described in claim 1 and loading plants essential oil antibacterial powder, which is characterized in that
The following steps are included:
(1) it prepares modified montmorillonite used: montmorillonite original powder being added in appropriate distilled water and is dispersed with stirring, add montmorillonite cation
3~12h, centrifugation or pumping are vibrated in the cetyl trimethylammonium bromide that 0.75~1.5 times of exchange capacity, 40~80 DEG C of condition water-baths
Filter separates solid liquid phase, and solid phase is washed with distilled water 3~5 times, and then dry at 40~80 DEG C, grinding obtains modified cover and takes off
Mountain flour；
(2) it loads plants essential oil: smectite powder obtained by step (1) being added in 50% ethanol solution and is stirred, is modified
Montmorillonite dispersion liquid, then be in mass ratio load plants essential oil: modified montmorillonite used=1:(1~2) addition plants essential oil, 40~60
DEG C condition water-bath oscillation 12~for 24 hours, centrifugation or filters separation solid liquid phase, and solid phase is washed 3~5 times with 50% ethanol solution,
Then dry at 40~60 DEG C, it grinds to obtain the final product modified montmorillonite used and loads plants essential oil antibacterial powder.
5. preparation method that is modified montmorillonite used as claimed in claim 4 and loading plants essential oil antibacterial powder, which is characterized in that described
Plants essential oil is one or more of carvacrol, Thymol and cinnamic acid.
6. preparation method that is modified montmorillonite used as claimed in claim 4 and loading plants essential oil antibacterial powder, which is characterized in that described
Montmorillonite original powder purity in step (1) is >=95%.
7. preparation method that is modified montmorillonite used as claimed in claim 4 and loading plants essential oil antibacterial powder, which is characterized in that described
Montmorillonite original powder cation exchange capacity in step (1) is 80~150mmol/100g.
8. preparation method that is modified montmorillonite used as claimed in claim 4 and loading plants essential oil antibacterial powder, which is characterized in that described
The amount of cetyl trimethylammonium bromide is 1.5 times of montmorillonite cation exchange capacity in step (1), and water-bath vibration temperature is
80 DEG C, time 3h, drying temperature is 60 DEG C.
9. modified montmorillonite used as claimed in claim 4 and load the preparation method of plants essential oil antibacterial powder, plant essence in step (2)
Oily and modified montmorillonite used mass ratio is 1:1.5, and water-bath vibration temperature is 60 DEG C, and the time is that for 24 hours, drying temperature is 40 DEG C.
10. preparation method that is modified montmorillonite used as claimed in claim 4 and loading plants essential oil antibacterial powder, which is characterized in that institute
Stating step (1) grind size is 200~300 mesh, and step (2) grind size is 200~300 mesh.
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