CN110433741A - Aromatic antibacterial microcapsule with carbon skeleton and preparation method thereof - Google Patents
Aromatic antibacterial microcapsule with carbon skeleton and preparation method thereof Download PDFInfo
- Publication number
- CN110433741A CN110433741A CN201910608647.5A CN201910608647A CN110433741A CN 110433741 A CN110433741 A CN 110433741A CN 201910608647 A CN201910608647 A CN 201910608647A CN 110433741 A CN110433741 A CN 110433741A
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- China
- Prior art keywords
- carbon skeleton
- gelatin
- microcapsule
- essential oil
- solution
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000003094 microcapsule Substances 0.000 title claims abstract description 56
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 23
- 125000003118 aryl group Chemical group 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 108010010803 Gelatin Proteins 0.000 claims abstract description 28
- 239000008273 gelatin Substances 0.000 claims abstract description 28
- 229920000159 gelatin Polymers 0.000 claims abstract description 28
- 235000019322 gelatine Nutrition 0.000 claims abstract description 28
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 28
- 239000000341 volatile oil Substances 0.000 claims abstract description 27
- 235000010489 acacia gum Nutrition 0.000 claims abstract description 14
- 239000001785 acacia senegal l. willd gum Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 41
- 239000000243 solution Substances 0.000 claims description 33
- 239000002245 particle Substances 0.000 claims description 26
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 239000006210 lotion Substances 0.000 claims description 19
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 241000218636 Thuja Species 0.000 claims description 14
- 235000008109 Thuja occidentalis Nutrition 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000004132 cross linking Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 238000005253 cladding Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 241000196324 Embryophyta Species 0.000 claims description 9
- 239000003638 chemical reducing agent Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- ZDXPYRJPNDTMRX-UHFFFAOYSA-N glutamine Natural products OC(=O)C(N)CCC(N)=O ZDXPYRJPNDTMRX-UHFFFAOYSA-N 0.000 claims description 7
- 241000220317 Rosa Species 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000003995 emulsifying agent Substances 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 5
- 240000001549 Ipomoea eriocarpa Species 0.000 claims description 4
- 235000005146 Ipomoea eriocarpa Nutrition 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 241000234435 Lilium Species 0.000 claims description 3
- 244000242564 Osmanthus fragrans Species 0.000 claims description 3
- 235000019083 Osmanthus fragrans Nutrition 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 235000005979 Citrus limon Nutrition 0.000 claims description 2
- 244000131522 Citrus pyriformis Species 0.000 claims description 2
- 235000018958 Gardenia augusta Nutrition 0.000 claims description 2
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical group OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 2
- 239000006071 cream Substances 0.000 claims description 2
- 230000001804 emulsifying effect Effects 0.000 claims description 2
- 239000000284 extract Substances 0.000 claims description 2
- 239000012065 filter cake Substances 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- 125000000404 glutamine group Chemical group N[C@@H](CCC(N)=O)C(=O)* 0.000 claims description 2
- 239000000171 lavandula angustifolia l. flower oil Substances 0.000 claims description 2
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 claims description 2
- 239000007968 orange flavor Substances 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000002242 deionisation method Methods 0.000 claims 1
- 238000004945 emulsification Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 14
- 239000011162 core material Substances 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 11
- 238000005354 coacervation Methods 0.000 abstract description 2
- 239000003431 cross linking reagent Substances 0.000 abstract description 2
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000000151 deposition Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000011068 loading method Methods 0.000 abstract 1
- 231100000956 nontoxicity Toxicity 0.000 abstract 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 11
- 229910052709 silver Inorganic materials 0.000 description 11
- 239000004332 silver Substances 0.000 description 11
- 239000000839 emulsion Substances 0.000 description 9
- 206010011732 Cyst Diseases 0.000 description 8
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 8
- 239000002775 capsule Substances 0.000 description 8
- 208000031513 cyst Diseases 0.000 description 8
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 8
- 235000013339 cereals Nutrition 0.000 description 6
- 239000003292 glue Substances 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- 101710134784 Agnoprotein Proteins 0.000 description 4
- 238000013019 agitation Methods 0.000 description 4
- 230000000845 anti-microbial effect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000003205 fragrance Substances 0.000 description 4
- 239000012437 perfumed product Substances 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- 238000013268 sustained release Methods 0.000 description 4
- 239000012730 sustained-release form Substances 0.000 description 4
- 230000003115 biocidal effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000352 supercritical drying Methods 0.000 description 3
- 210000000988 bone and bone Anatomy 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 229920005615 natural polymer Polymers 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 241000218691 Cupressaceae Species 0.000 description 1
- 229920000858 Cyclodextrin Polymers 0.000 description 1
- 239000001116 FEMA 4028 Substances 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 240000002924 Platycladus orientalis Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 description 1
- 235000011175 beta-cyclodextrine Nutrition 0.000 description 1
- 229960004853 betadex Drugs 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000001935 peptisation Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- 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
- A01N25/26—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 in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
-
- 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
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L9/00—Disinfection, sterilisation or deodorisation of air
- A61L9/01—Deodorant compositions
- A61L9/012—Deodorant compositions characterised by being in a special form, e.g. gels, emulsions
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L9/00—Disinfection, sterilisation or deodorisation of air
- A61L9/01—Deodorant compositions
- A61L9/013—Deodorant compositions containing animal or plant extracts, or vegetable material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/10—Complex coacervation, i.e. interaction of oppositely charged particles
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2209/00—Aspects relating to disinfection, sterilisation or deodorisation of air
- A61L2209/20—Method-related aspects
- A61L2209/21—Use of chemical compounds for treating air or the like
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Zoology (AREA)
- Pest Control & Pesticides (AREA)
- Dentistry (AREA)
- Environmental Sciences (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- Organic Chemistry (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Dispersion Chemistry (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Botany (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Toxicology (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention provides a fragrant antibacterial microcapsule with a carbon skeleton and a preparation method thereof, wherein essence essential oil is used as a core material, natural high-molecular gelatin and Arabic gum are used as wall materials, and a complex coacervation method is adopted to prepare the fragrant microcapsule with the carbon skeleton and the antibacterial property; firstly, plant pollen is calcined into a hollow carbon skeleton after being processed, and then silver nano-particles are loaded on the surface of the carbon skeleton by a sol loading method; then, dispersing and coating the core material essence essential oil in the hollow carbon skeleton; finally, gradually depositing the gelatin and the Arabic gum on the surface of the carbon skeleton to embed the core material, and adding a cross-linking agent for curing to form the long-acting slow-release aromatic antibacterial microcapsule with a stable structure; the carbon skeleton microcapsule prepared by the invention has aromatic smell and antibacterial performance, has the characteristics of environmental protection, no toxicity, slow release, bacteriostasis, good mechanical strength, good heat resistance and the like, improves the application stability of the essence microcapsule, and prolongs the service life.
Description
(1) technical field
The present invention relates to a kind of microcapsules and preparation method thereof with aromatic odor and anti-microbial property, especially a kind of tool
There is the aromatic antibacterial microcapsule and preparation method thereof of carbon skeleton supporting layer, belongs to Micro-Encapsulation Technique field.
(2) background technique
With the development of economy, social progress, the life style and living environment of the mankind all have changed a lot.
Requirement of the people to extensive stock is also from past practical to decoration, enjoyment, health conversion.It does not require nothing more than and visually obtains
Beautiful enjoyment is obtained, also pursues and obtains pleasant satisfaction in smell.Perfumed products with various aromatic odor quietly rise,
Intense strain, pressure relief and the effects of urge people excited it is found that fragrance is releived.The storage of essence and stabilization are that flavoring produces
Product whether can Longaacting fragrance-aretaining it is crucial, most of component in essence has very strong volatility, to outside stimulus, such as light, heat,
Oxygen is sensitive, easily with other substance reactions, to gradually fail, for require the product of durable aroma directly apply essence flavoring without
Method is met the requirements.Microcapsules technology is that a kind of solid or liquid are coated with filmogen makes to form the technology of fine particle, will
Essence microcapsuleization can provide a protective shell to essence, shield it and contact with outside air or the direct of product,
Effectively the volatilization of essence is prevented, reacts or is diffused into perfumed products.Overwhelming majority perfumed products all use this at present
Kind technology.
Although microcapsules technology can be good at storing essence, prevent its volatilization loss, but existing microcapsules are in reality
Still there are some problems in the application of border, for example is easy broken capsule on a large scale in the processing and forming or subsequent processing of perfumed products and leads
Cause essence loss.Patent CN103849466A is successively coated outside capsule-core from the inside to the outside using oil soluble perfume essential oil as capsule-core
There are first layer wall material, second layer wall material and third layer wall material, so that microcapsules capsule material is firm, does not occur to advise greatly in extrusion process
Mould breaks capsule.Although improving the leakproofness of essential oil in this way, cyst wall is excessively fine and close to be difficult the fragrance of essential oil capsule-core from glue
It is released in capsule, and three layers of cyst wall encapsulation increase process complexity, the production cycle is long, is unfavorable for industrialized production.Specially
Sharp CN102630705A is prepared for having receiving for anti-microbial property using beta-cyclodextrin using oil solubility nanometer ag material as core material as wall material
The silver-colored microcapsule anti-bacterial agent of rice, the method that drying process uses supercritical drying avoid the contraction of microcapsules in the drying process
And collapsing, improve agglomeration traits when preparing nano-powder drying.But supercritical drying need to use autoclave, autoclave is close
Envelope property requires high.And the experimental period that supercritical drying process needs is relatively long, and low output is at high cost.
(3) summary of the invention
The object of the present invention is to provide a kind of carbon skeleton microcapsules for having both aromatic odor and anti-microbial property, have environmentally friendly nothing
The features such as poison, antibacterial, mechanical strength is good, heat-resist sustained release, the stability of essence microcapsule application is improved, use is extended
Service life.
For the present invention using essence essential oil as core material, natural polymer gelatin and Arabic gum are wall material, using complex coacervation come
Prepare the carbon skeleton aromatic micro-capsule with antibiotic property.Firstly, the pollen of plant is sintered into hollow carbon skeleton after processing,
Again by colloidal sol load method in carbon skeleton area load silver nano-grain；Then core material essence essential oil dispersion is coated on hollow carbon
In skeleton；Finally, gelatin and Arabic gum are gradually deposited at carbon skeleton surface and embed core material, and it is solid that crosslinking agent is added
Change, forms the long-acting slow-release aromatic antibacterial microcapsule with rock-steady structure.
Technical scheme is as follows:
A kind of aromatic antibacterial microcapsule with carbon skeleton, is prepared as follows to obtain:
(1) plant pollen is taken, 1~3h is impregnated with the mixed solution of first alcohol and water, then under 80~100 DEG C of vacuum conditions
Pollen grain after drying is then calcined 2~4h at 200~500 DEG C, hollow carbon skeleton is made by drying in nitrogen atmosphere
Grain；
The plant pollen is lilium pollen, sweet osmanthus pollen or morning glory pollen；
The volume ratio of methanol and water is 1~4:1 in the mixed solution of the first alcohol and water；
The volumetric usage of the mixed solution of the first alcohol and water is calculated as 30~50mL/g with the quality of plant pollen；
(2) by AgNO3Aqueous solution, reducing agent, water mixing, are added hollow carbon skeleton particle obtained by step (1), 60~
150 DEG C (preferably 90 DEG C) are stirred to react 1~3h (preferably 2h), filter, filtration cakes torrefaction (60~80 DEG C, 8~12h), and load silver is made
Hollow carbon skeleton particle；
The AgNO3The mass ratio of contained elements A g and hollow carbon skeleton particle is 0.5~2:100 in aqueous solution；
The size that gained carries the silver nano-grain of silver-colored hollow carbon skeleton particle load is 5~20nm；
The AgNO3The concentration of aqueous solution is 0.1mol/L；
The reducing agent is arbor-vitae (scientific name: Platycladus orientalis (L.) Franco) extracting solution, the side
Cypress extracting solution the preparation method comprises the following steps: arbor-vitae leaf dried powder is add to deionized water, stir 12h at 25 DEG C, filtered through filter paper
Gained filtrate is arbor-vitae extracting solution；The volumetric usage of the deionized water is calculated as 5mL/g with the quality of arbor-vitae leaf dried powder；
The AgNO3Aqueous solution, reducing agent, water 0.015~0.025:1 of volume ratio~1.5:1；
At (3) 40 DEG C, gelatin is dissolved in deionized water and is configured to gelatin solution (1~3wt%)；At 40 DEG C, by me
Primary peptization is configured to gumwater (1~3wt%) in deionized water；
(4) essence essential oil is taken, is added obtained by step (2) and carries silver-colored hollow carbon skeleton particle, 2000~10000r/min's
5~15min is stirred under rate, and the lotion of carbon skeleton cladding essence essential oil is made；
The essence essential oil in flavoring rose essence, cream jasmin france, lemon extract, lavender oil, orange flavor one
Kind or two kinds；
(5) gelatin solution and gumwater prepared in step (3) are uniformly mixed, carbon obtained by step (4) is added
Skeleton coats the lotion and emulsifier of essence essential oil, and 20~40min of stirring and emulsifying under 2000~10000r/min rate is formed
Stable emulsion；
The mass ratio of the gelatin and Arabic gum is 1:0.3~3, preferably 1:1；
In the lotion of the carbon skeleton cladding essence essential oil quality of essence essential oil and gelatin and Arabic gum gross mass it
Than for 1~6:1；
The quality and the ratio between gelatin and Arabic gum gross mass of carbon skeleton in the lotion of the carbon skeleton cladding essence essential oil
For 1:5~20；
The emulsifier is lauryl sodium sulfate, and the dosage of the emulsifier is the 1~3% of the step system gross mass；
(6) stirring rate is adjusted to 600r/min, extremely with the pH of lotion in acetic acid aqueous solution (10wt%) regulating step (5)
4.0~5.0,15~30min is reacted at 40~50 DEG C, is then cooled to 0~10 DEG C, fast insulated and stirred 1h is stirred in holding, then
With NaOH aqueous solution (10wt%) adjust pH to 7.0, be added crosslinking and curing agent, holding stir speed continue insulated and stirred reaction 10~
16h is filtered later, and Washing of Filter Cake (uses deionized water), is freeze-dried to get the micro- glue of the fragrant antimicrobial with carbon skeleton
Capsule；
The crosslinking and curing agent is glutamine transaminage, and the dosage of the crosslinking and curing agent is that gelatin and Arabic gum are total
1~3 times of quality.
The present invention utilizes the design feature of plant pollen, forms the carbon skeleton with hollow structure by calcining, is planted
Enter microcapsules as supporting layer, template action is not only played in microcapsules forming process, but also improves the machine of microcapsules
Tool intensity, efficiently solve microcapsules drying, product processing and forming or subsequent processes in there is extensive collapse
Or the problem of broken capsule, the structural stability of microcapsules in the application is maintained well, so that the fragrance for improving microcapsules is slow
Release performance.Application range has been expanded with microcapsules prepared by this method, there is very big application potential.
The present invention is reducing agent by Ag using arbor-vitae extracting solution+It is reduced into Ag nano particle and is supported on carbon skeleton surface, assign
Microcapsules broad spectrum antibacterial performance is given, and Ag nano particle is covered by the cyst wall of microcapsules, it is de- not only to effectively prevent it
Loss is fallen, the performance of nanometer Ag sustained release, durable antibiotic and fastness is also improved.
For the present invention using natural polymer gelatin and Arabic gum as wall material, essence essential oil is core material, is prepared with plant pollen
Carbon skeleton be supporting layer, using glutamine transaminage as crosslinking and curing agent, raw materials used is nontoxic material, guarantee
The safety of microcapsules application.
There is the present invention aromatic antibacterial microcapsule of carbon skeleton can be applied to leather and fur products, and smoking article and textile fabric add
In perfume (or spice).
Compared with prior art, the present invention has the following obvious advantages:
(1) compared with traditional microcapsules, microcapsules of the invention have one layer of carbon skeleton supporting layer, not only contribute to micro-
The molding of capsule, and the mechanical strength of microcapsules is improved, avoid traditional microcapsules from occurring big rule in application and use process
Mould collapses and broken capsule phenomenon, extends the service life of microcapsules, improves sustained release performance.
(2) present invention has also loaded one layer of Ag nano particle using carbon skeleton on it, so that microcapsules have fragrance
Also there is broad spectrum antibacterial performance while smell, expanded the application range of microcapsules, have and greatly apply potential quality.And carbon
Ag nano particle on skeleton is coated in effect microcapsule wall, effectively prevents its loss that falls off, improve nanometer Ag sustained release and
Durable antibiotic performance.
(3) the raw materials used present invention is environment-protecting and non-poisonous material, use is safe, from a wealth of sources, and cost is relatively low, technique letter
It is single, it is suitable for industrialized production.
(4) Detailed description of the invention
A, B are respectively the spherical shape prepared, elliposoidal microcapsule structure schematic diagram in Fig. 1；
In figure: the essence essential oil capsule-core of 1- microcapsules；2- carbon skeleton；3-Ag nano particle；4- cyst wall.
Fig. 2 is the scanning electron microscope (SEM) photograph of microcapsules prepared by embodiment 1.
(5) specific embodiment
Combined with specific embodiments below, the invention will be further described, but the present invention is not limited to the following example, In
It does not depart from the content of present invention and range, change all should be comprising within the technical scope of the present invention.
Embodiment 1
(1) 10g lilium pollen is taken, the methanol and water mixed solution 400mL for being 3:1 with volume ratio impregnate 2h, and at 80 DEG C
It is dried under vacuum condition, the pollen grain after drying is then calcined into 2h in nitrogen atmosphere at 400 DEG C, hollow carbon skeleton is made
Particle；
(2) AgNO of the 0.1mol/L of 190 μ L is taken3Conical flask is added in solution and 10mL water and 15mL arbor-vitae extracting solution
In, and the carbon skeleton particle being added in 0.1g (1), under the conditions of 90 DEG C of oil baths, magnetic agitation reacts 2h, filters, and does at 80 DEG C
The hollow carbon skeleton particle for carrying silver is made in dry 12h；
(3) 1g gelatin is taken, 100mL deionized water is added, dissolves it sufficiently in 40 DEG C of water-baths；Separately take 1g Arabic
Glue is added 100mL deionized water, dissolves it sufficiently；
(4) 6g flavoring rose essence is taken, the load silver hollow carbon skeleton particle 0.1g dried in (2) is added, 10000r/min's
10min is stirred under mixing speed, the lotion of carbon skeleton cladding essence essential oil is made；
(5) by (3) gelatin solution and gumwater be uniformly mixed, be added (4) in lotion and 2g dodecane
Base sodium sulphate persistently emulsifies 30min under the conditions of 10000r/min, makes to be sufficiently mixed uniformly, forms stable emulsion；
(6) mixing speed is reduced to 600r/min, adjusts ph value of emulsion in (5) with the acetic acid solution that mass fraction is 10%
To 4.2,15min is reacted under 42 DEG C of water-baths, is then transferred in ice bath, makes temperature decrease to 5 DEG C, 1h is kept the temperature and keeps low speed
Then stirring adjusts pH to 7.0 with the NaOH solution that mass fraction is 10%, 2g glutamine transaminage is added, keeps low temperature
Reaction 12h is stirred at low speed, cyst wall crosslinking curing is made.After the reaction was completed, it filters, is washed with deionized, then freeze-drying is
Solid microcapsules are obtained, Fig. 2 is product scanning electron microscope (SEM) photograph.
Embodiment 2
(1) 10g sweet osmanthus pollen is taken, the methanol and water mixed solution 400mL for being 3:1 with volume ratio impregnate 2h, and at 80 DEG C
It is dried under vacuum condition, the pollen grain after drying is then calcined into 3h in nitrogen atmosphere at 300 DEG C, hollow carbon skeleton is made
Particle；
(2) AgNO of the 0.1mol/L of 380 μ L is taken3Conical flask is added in solution and 15mL water and 20mL arbor-vitae extracting solution
In, and the carbon skeleton particle being added in 0.2g (1), under the conditions of 90 DEG C of oil baths, magnetic agitation reacts 2h, filters, and does at 80 DEG C
The hollow carbon skeleton particle for carrying silver is made in dry 12h；
(3) 1g gelatin is taken, 100mL deionized water is added, dissolves it sufficiently in 40 DEG C of water-baths；Separately take 1g Arabic
Glue is added 100mL deionized water, dissolves it sufficiently；
(4) 8g flavoring rose essence is taken, the load silver hollow carbon skeleton particle 0.2g dried in (2) is added, 10000r/min's
15min is stirred under mixing speed, the lotion of carbon skeleton cladding essence essential oil is made；
(5) by (3) gelatin solution and gumwater be uniformly mixed, be added (4) in lotion and 3g dodecane
Base sodium sulphate persistently emulsifies 35min under the conditions of 10000r/min, makes to be sufficiently mixed uniformly, forms stable emulsion；
(6) mixing speed is reduced to 600r/min, adjusts ph value of emulsion in (5) with the acetic acid solution that mass fraction is 10%
To 4.3,15min is reacted under 44 DEG C of water-baths, is then transferred in ice bath, makes temperature decrease to 5 DEG C, 1h is kept the temperature and keeps low speed
Then stirring adjusts pH to 7.0 with the NaOH solution that mass fraction is 10%, 3g glutamine transaminage is added, keeps low temperature
Reaction 12h is stirred at low speed, cyst wall crosslinking curing is made.After the reaction was completed, it filters, is washed with deionized, then freeze-drying is
Obtain solid microcapsules.
Embodiment 3
(1) 10g morning glory pollen is taken, the methanol and water mixed solution 400mL for being 3:1 with volume ratio impregnate 2h, and 80
It is dried under DEG C vacuum condition, the pollen grain after drying is then calcined into 4h in nitrogen atmosphere at 200 DEG C, hollow carbon bone is made
Frame particle；
(2) AgNO of the 0.1mol/L of 247 μ L is taken3Conical flask is added in solution and 12mL water and 12mL arbor-vitae extracting solution
In, and the carbon skeleton particle being added in 0.13g (1), under the conditions of 90 DEG C of oil baths, magnetic agitation reacts 2h, filters, and does at 80 DEG C
The hollow carbon skeleton particle for carrying silver is made in dry 12h；
(3) 1g gelatin is taken, 100mL deionized water is added, dissolves it sufficiently in 40 DEG C of water-baths；Separately take 1g Arabic
Glue is added 100mL deionized water, dissolves it sufficiently；
(4) 10g flavoring rose essence is taken, the load silver hollow carbon skeleton particle 0.13g dried in (2) is added, in 10000r/min
Mixing speed under stir 15min, be made carbon skeleton cladding essence essential oil lotion；
(5) by (3) gelatin solution and gumwater be uniformly mixed, be added (4) in lotion and 4g dodecane
Base sodium sulphate persistently emulsifies 35min under the conditions of 10000r/min, makes to be sufficiently mixed uniformly, forms stable emulsion；
(6) mixing speed is reduced to 600r/min, adjusts ph value of emulsion in (5) with the acetic acid solution that mass fraction is 10%
To 4.4,15min is reacted under 46 DEG C of water-baths, is then transferred in ice bath, makes temperature decrease to 5 DEG C, 1h is kept the temperature and keeps low speed
Then stirring adjusts pH to 7.0 with the NaOH solution that mass fraction is 10%, 4g glutamine transaminage is added, keeps low temperature
Reaction 14h is stirred at low speed, cyst wall crosslinking curing is made.After the reaction was completed, it filters, is washed with deionized, then freeze-drying is
Obtain solid microcapsules.
Embodiment 4
(1) 10g morning glory pollen is taken, the methanol and water mixed solution 400mL for being 3:1 with volume ratio impregnate 2h, and 80
It is dried under DEG C vacuum condition, the pollen grain after drying is then calcined into 2h in nitrogen atmosphere at 300 DEG C, hollow carbon bone is made
Frame particle；
(2) AgNO of the 0.1mol/L of 760 μ L is taken3Conical flask is added in solution and 30mL water and 40mL arbor-vitae extracting solution
In, and the carbon skeleton particle being added in 0.4g (1), under the conditions of 90 DEG C of oil baths, magnetic agitation reacts 2h, filters, and does at 80 DEG C
The hollow carbon skeleton particle for carrying silver is made in dry 12h；
(3) 1g gelatin is taken, 100mL deionized water is added, dissolves it sufficiently in 40 DEG C of water-baths；Separately take 1g Arabic
Glue is added 100mL deionized water, dissolves it sufficiently；
(4) 12g flavoring rose essence is taken, the load silver hollow carbon skeleton particle 0.4g dried in (2) is added, 10000r/min's
15min is stirred under mixing speed, the lotion of carbon skeleton cladding essence essential oil is made；
(5) by (3) gelatin solution and gumwater be uniformly mixed, be added (4) in lotion and 5g dodecane
Base sodium sulphate persistently emulsifies 35min under the conditions of 10000r/min, makes to be sufficiently mixed uniformly, forms stable emulsion；
(6) mixing speed is reduced to 600r/min, adjusts ph value of emulsion in (5) with the acetic acid solution that mass fraction is 10%
To 4.5,15min is reacted under 48 DEG C of water-baths, is then transferred in ice bath, makes temperature decrease to 5 DEG C, 1h is kept the temperature and keeps low speed
Then stirring adjusts pH to 7.0 with the NaOH solution that mass fraction is 10%, 5g glutamine transaminage is added, keeps low temperature
Reaction 16h is stirred at low speed, cyst wall crosslinking curing is made.After the reaction was completed, it filters, is washed with deionized, then freeze-drying is
Obtain solid microcapsules.
Claims (9)
1. a kind of aromatic antibacterial microcapsule with carbon skeleton, which is characterized in that be prepared as follows to obtain:
(1) plant pollen is taken, 1~3h is impregnated with the mixed solution of first alcohol and water, is then dried under 80~100 DEG C of vacuum conditions
It is dry, the pollen grain after drying is then calcined in nitrogen atmosphere to 2~4h at 200~500 DEG C, hollow carbon skeleton particle is made；
The volume ratio of methanol and water is 1~4:1 in the mixed solution of the first alcohol and water；
(2) by AgNO3Aqueous solution, reducing agent, water mixing, are added hollow carbon skeleton particle obtained by step (1), stir at 60~150 DEG C
1~3h of reaction is mixed, is filtered, filtration cakes torrefaction, the silver-colored hollow carbon skeleton particle of load is made；
The AgNO3The mass ratio of contained elements A g and hollow carbon skeleton particle is 0.5~2:100 in aqueous solution；
The reducing agent is arbor-vitae extracting solution；
At (3) 40 DEG C, gelatin is dissolved in deionized water and is configured to gelatin solution；At 40 DEG C, Arabic gum is dissolved in deionization
Gumwater is configured in water；
(4) essence essential oil is taken, is added obtained by step (2) and carries silver-colored hollow carbon skeleton particle, in the rate of 2000~10000r/min
The lotion of carbon skeleton cladding essence essential oil is made in 5~15min of lower stirring；
(5) gelatin solution and gumwater prepared in step (3) are uniformly mixed, carbon skeleton obtained by step (4) is added
The lotion and emulsifier of essence essential oil are coated, 20~40min of stirring and emulsifying under 2000~10000r/min rate is formed and stablized
Lotion；
The mass ratio of the gelatin and Arabic gum is 1:0.3~3；
The quality of essence essential oil and the ratio between gelatin and Arabic gum gross mass are 1 in the lotion of the carbon skeleton cladding essence essential oil
~6:1；
The quality of carbon skeleton and the ratio between gelatin and Arabic gum gross mass are 1:5 in the lotion of the carbon skeleton cladding essence essential oil
~20；
The emulsifier is lauryl sodium sulfate；
(6) stirring rate is adjusted to 600r/min, with the pH to 4.0~5.0, In of lotion in acetic acid aqueous solution regulating step (5)
15~30min is reacted at 40~50 DEG C, is then cooled to 0~10 DEG C, and fast insulated and stirred 1h is stirred in holding, then uses NaOH aqueous solution
PH to 7.0 is adjusted, crosslinking and curing agent is added, holding stirs speed continuation insulated and stirred and reacts 10~16h, filters later, Washing of Filter Cake,
Freeze-drying is to get the aromatic antibacterial microcapsule with carbon skeleton；
The crosslinking and curing agent is glutamine transaminage.
2. as described in claim 1 with the aromatic antibacterial microcapsule of carbon skeleton, which is characterized in that in step (1), the plant
Pollen is lilium pollen, sweet osmanthus pollen or morning glory pollen.
3. as described in claim 1 with the aromatic antibacterial microcapsule of carbon skeleton, which is characterized in that in step (1), the methanol
30~50mL/g is calculated as with the quality of plant pollen with the volumetric usage of the mixed solution of water.
4. as described in claim 1 with the aromatic antibacterial microcapsule of carbon skeleton, which is characterized in that in step (2), the AgNO3
The concentration of aqueous solution is 0.1mol/L；
The reducing agent arbor-vitae extracting solution the preparation method comprises the following steps: arbor-vitae leaf dried powder is add to deionized water, stirred at 25 DEG C
12h is mixed, filtering gained filtrate through filter paper is arbor-vitae extracting solution；The volumetric usage of the deionized water is with the matter of arbor-vitae leaf dried powder
Amount is calculated as 5mL/g；
The AgNO3Aqueous solution, reducing agent, water 0.015~0.025:1 of volume ratio~1.5:1.
5. as described in claim 1 with the aromatic antibacterial microcapsule of carbon skeleton, which is characterized in that in step (3), the gelatin
The concentration of solution is 1~3wt%.
6. as described in claim 1 with carbon skeleton aromatic antibacterial microcapsule, which is characterized in that in step (3), it is described I
The concentration of primary sol solution is 1~3wt%.
7. as described in claim 1 with the aromatic antibacterial microcapsule of carbon skeleton, which is characterized in that in step (4), the essence
Essential oil is selected from one or both of flavoring rose essence, cream jasmin france, lemon extract, lavender oil, orange flavor.
8. as described in claim 1 with the aromatic antibacterial microcapsule of carbon skeleton, which is characterized in that in step (5), the emulsification
The dosage of agent is the 1~3% of the step system gross mass.
9. as described in claim 1 with the aromatic antibacterial microcapsule of carbon skeleton, which is characterized in that in step (6), the crosslinking
The dosage of curing agent is 1~3 times of gelatin and Arabic gum gross mass.
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