CN109183173A - A kind of fibroin albumen doughnut of the microcapsules containing wormwood and preparation method thereof - Google Patents
A kind of fibroin albumen doughnut of the microcapsules containing wormwood and preparation method thereof Download PDFInfo
- Publication number
- CN109183173A CN109183173A CN201811268535.1A CN201811268535A CN109183173A CN 109183173 A CN109183173 A CN 109183173A CN 201811268535 A CN201811268535 A CN 201811268535A CN 109183173 A CN109183173 A CN 109183173A
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- China
- Prior art keywords
- wormwood
- doughnut
- microcapsules
- fibroin albumen
- essential oil
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Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F4/00—Monocomponent artificial filaments or the like of proteins; Manufacture thereof
- D01F4/02—Monocomponent artificial filaments or the like of proteins; Manufacture thereof from fibroin
-
- 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
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/02—Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Textile Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Mechanical Engineering (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Cosmetics (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses fibroin albumen doughnuts of a kind of microcapsules containing wormwood and preparation method thereof, its key points of the technical solution are that: a kind of fibroin albumen doughnut of the microcapsules containing wormwood, it is characterized in that, fibroin albumen doughnut including being in hollow setting, several wormwood microcapsules are provided in the cavity of the fibroin albumen doughnut, wormwood essential oil is provided in the wormwood microcapsules, the wormwood microcapsules are freeze-dried after complex coacervation by gum arabic, gelatin, wormwood essential oil and are made.The present invention reaches the volatilization for slowing down wormwood essential oil, and expands wormwood essential oil application surface.
Description
Technical field
The invention belongs to function textile field, more particularly to a kind of fibroin albumen doughnut of microcapsules containing wormwood
And preparation method thereof.
Background technique
It reaches its maturity with technology, the multidisciplinary main flow direction for being combined into 21 century, by drug medicine in conjunction with textile
Using as current research hot spot.Intersecting and permeate due to subject, combines preparation with textile fabric for drug material
Function textile with excellent slow releasing health medicinal properties has become textile material field research boom.
Wormwood also known as moxibustion grass, composite family sagebruss.All herbal medicine has warming channel for arresting bleeding, warm channels and collaterals, moisture, cold dispelling is gone to stop
Bitterly, the effects of antiallergy, antibacterial anti-inflammatory, antiasthmatic-antitussive, folium artemisiae argyi is the part that wormwood is played effectiveness, Blumea oil, i.e. wormwood essential oil,
Wherein containing can stimulating central nervous system, antipyretic, hemostasis, the absynthol of analgesic activity, absinth ketone, fragrance has the work of expelling parasite
With.
However wormwood essential oil has volatile, effective time short disadvantage is not easy to make the popularization of wormwood essential oil product
With.
Therefore it needs to propose the new scheme of one kind to solve this problem.
Summary of the invention
In view of the above-mentioned problems, the object of the present invention is to provide a kind of fibroin albumen doughnut of microcapsules containing wormwood and its
Preparation method reaches the volatilization for slowing down wormwood essential oil, and expands wormwood essential oil application surface.
Above-mentioned technical purpose of the invention has the technical scheme that a kind of silk of microcapsules containing wormwood
Fibroin doughnut, which is characterized in that the fibroin albumen doughnut including being in hollow setting, the hollow fibre of fibroin albumen
It is provided with several wormwood microcapsules in the cavity of dimension, wormwood essential oil, the wormwood microcapsules are provided in the wormwood microcapsules
It is freeze-dried and is made after complex coacervation by gum arabic, gelatin, wormwood essential oil.
Further, the wormwood Microcapsules Size is 50~1200nm.
Further, the wormwood Microcapsules Size is 100~500nm.
Further, the preparation method of the fibroin albumen doughnut of a kind of microcapsules containing wormwood, includes the following steps:
Step 1, gum arabic and Gelatin are added dropwise wormwood essential oil and are emulsified with dispersing agent in deionized water；
Step 2, the pH value that the solution after emulsification is adjusted to solution with acetum, reach PH=3-4, carry out multiple agglomerated
Journey makes capsule material be coated on essential oil surface；
Solution after step 3, multiple cohesion is cooled under 0 DEG C of environment through stirring in blender, uses sodium hydroxide solution
It adjusts, reaches the PH=9-10 of solution, carry out low temperature alkalization；
The 25% glutaraldehyde stirring that volume ratio is 10ml/l is added after solution to be replied to room temperature in step 4, adds tannic acid
And stir, wormwood microscapsule powder is obtained after freeze-drying, wormwood microcapsules are dispersed in water, mass fraction is made is 18%
~22% dispersion liquid；
Silk is placed in sodium carbonate liquor and removes silk gum by step 5, obtains fibroin, then molten with the mixing of potassium bromide/ethyl alcohol
Fibroin is dissolved in agent, obtains fibroin albumen spinning solution；
Spinning solution is spun into fibroin albumen doughnut with hollow fiber spinning device by step 6, then fibroin albumen is hollow
Wormwood micro-capsule dispersion liquid, the rubber tube of other end access opening are immersed in fiber one end, and rubber tube connects vacuum pump, passes through vacuum
Pump is evacuated to fibroin albumen doughnut upper end and liquid occurs, and vacuum pump is closed；
The doughnut for filling dispersion liquid is freeze-dried by step 7, removes the moisture in dispersion liquid, and wormwood essential oil is micro-
Capsule is deposited in fibroin albumen doughnut chamber.
Further, in step 1, mass fraction is 3.8~4.2% to the gum arabic in deionized water, gelatin
Mass fraction is 3.8~4.2%, and solution temperature is 40 DEG C, and wormwood essential oil mass fraction 11.8~12.2% stirs 30 minutes,
10000 revs/min of stirring 20s, stir 15 minutes, dispersing agent are then added while stirring by 3000~4000 revs/min.
Further, in step 2, acetum used in PH, mass fraction 10%, stirring are adjusted before solution agglomerates again
Rate is 3000-4000 revs/min, and the reaction time is 30 minutes.
Further, in step 3, solution is gradually cooled to 0~5 DEG C after multiple cohesion, temperature reach after with 10% hydroxide
It is 9--10 that sodium solution, which adjusts PH, and temperature is kept for 5 DEG C hereinafter, speed of agitator is 2000-3000 revs/min, and mixing time is 20 points
Clock.
Further, in step 4,25% glutaraldehyde volume ratio is 10ml/l, and mixing time is 30 minutes；Move on to 40 DEG C of perseverances
In warm water bath, mixing time 3h；Adding tannic acid usage ratio is 10g/l, mixing time 4.5h.By the body after solidification
It ties up under the conditions of revolving speed is 5000 revs/min and is centrifuged 10min, freeze-drying obtains wormwood microscapsule powder.
Further, in steps of 5, silk boils 30min in the ratio bath raio of 1:20 in the sodium carbonate liquor of 500g/l,
It is repeated 3 times, fibroin is cleaned with 60 DEG C of deionized water after degumming, is then dried with baking oven.The bromine for being 42:58 with mass ratio
Change potassium and dehydrated alcohol is mixed into solvent at 80 DEG C, dissolve fibroin, at room temperature dipping expansion 6-8 hours.
Compared with prior art, present invention has the advantage that
1) present invention is handled wormwood essential oil using microencapsulation technology, is wrapped in essential oil in capsule material, is formed
Microcapsules effectively extend essential oil diffusion time, enhance sustained release performance；Sufficiently solidification enhancing wormwood microcapsules physical property.
2) present invention assists vacuum filtration technology by diffusion to wormwood microcapsules, improves doughnut filling rate and micro-
Capsule utilization rate significantly promotes lasting medicine degree and sustained release performance.
3) for the present invention by being freeze-dried to the intracavitary dispersion liquid of doughnut, amplitude peak remains Chinese mugwort in fiber core
Careless microcapsules obtain powdered precipitating, improve medicine stability and fiber washing fastness in fiber.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of embodiment one；
Fig. 2 is the flow chart of embodiment two and embodiment three.
Specific embodiment
With reference to the accompanying drawings and examples, the present invention will be described in detail.
Embodiment one: a kind of fibroin albumen doughnut of the microcapsules containing wormwood, as shown in Figure 1, including is in hollow setting
Fibroin albumen doughnut 1, fibroin albumen doughnut 1 handled by natural silk degumming after after obtain, and in fibroin albumen
Setting has wormwood essential oil in wormwood microcapsules 2, wormwood essential oil can be saturating by several wormwood microcapsules 2 in the cavity of hollow fiber 1
Control fiber in wormwood microcapsules 2 and fibroin albumen is crossed slowly to evaporate into external environment.Wormwood microcapsules 2 by gum arabic,
Gelatin, wormwood essential oil are freeze-dried after complex coacervation to be made.And the micro- 50~1200nm of the partial size of wormwood microcapsules 2, preferably
For 100~500nm；The surface area that can guarantee wormwood microcapsules 2 in this way, is conducive to drug release, and lesser diameter facilitates spinning
Silk.
Wormwood essential oil in wormwood microcapsules 2 can be volatilized through the slight void or molecular gap of wormwood microcapsules 2
Come, and evaporated into external environment through fibroin albumen doughnut 1, passes through wormwood capsule and fibroin albumen doughnut in this way
1 plays the role of dual-sustained-release, thus reach and pull ring wormwood essential oil volatilization, extend wormwood essential oil action time.
Embodiment two: a kind of to be used to prepare a kind of fibroin albumen doughnut of the microcapsules containing wormwood described in embodiment one
Preparation method.It prepares as shown in Fig. 2, first carrying out wormwood microcapsules 2: first heating gum arabic and gelatin in 4% ratio
It is dissolved in deionized water, wormwood essential oil and dispersing agent is added, stir 40min, revolving speed 2000r/min, adjusted with 10% acetic acid
PH to 3 stirs 30min, revolving speed 2000r/min with magnetic stirrer, system is cooled to 1 DEG C, and at low ambient temperatures, is added
10% sodium hydroxide solution is 9 to PH, after blender stirring rate 2000r/min, mixing time 20min, replys room temperature and is added
25% glutaraldehyde stirs 3 hours and tannic acid stirs 4 hours, and it is 12 hours dry that drying machine is put into after stirring；To prepare
Wormwood microcapsules 2 are completed, and 2 partial size of wormwood microcapsules prepared is in for the section 100~500nm.
Then the preparation of fibroin albumen doughnut 1 is carried out again: by silk by 1:20's in the sodium carbonate liquor of 500g/l
Ratio bath raio boils 30min, is repeated 3 times, and fibroin is cleaned with 60 DEG C of deionized water after degumming, is then dried with baking oven.
The potassium bromide for being 42:58 with mass ratio and dehydrated alcohol are mixed into solvent at 80 DEG C, dissolve fibroin, at room temperature dipping expansion
6 hours.Fibroin albumen spinning solution is made, spinning solution is added in doughnut preparation facilities, it is hollow that silk fibroin is made
Fiber 1.
Wormwood microcapsules 2 are inserted later in the cavity of fibroin albumen doughnut 1: wormwood essential oil microcapsules are pressed 20%
Ratio, which is dispersed in water, is made dispersion, dispersion liquid is immersed in 1 one end of silk fibroin hollow fiber, other end access is opened
The rubber tube of mouth, the rubber tube other end connect vacuum pump, and vacuum pump is evacuated to fiber upper end and liquid occurs, vacuum pump closes
It closes.The doughnut freeze-drying that dispersion liquid will be filled, remove the moisture in dispersion liquid, and wormwood essential oil microcapsules are deposited in
In hollow fiber chamber.
The fibroin albumen doughnut of the microcapsules prepared by the above method containing wormwood, reaches and slows down in wormwood microcapsules 2
The volatilization of wormwood essential oil, and under normal temperature and pressure environment, wormwood essential oil volatilizees duration not 48 hours, i.e., using micro- containing wormwood
At the fibroin albumen doughnut of capsule 48 hours, remain to smell the distinctive fragrance of wormwood essential oil.
Embodiment three: a kind of to be used to prepare a kind of fibroin albumen doughnut of the microcapsules containing wormwood described in embodiment one
Preparation method.As shown in Fig. 2, first wormwood essential oil microcapsules preparation: first heating gum arabic and gelatin in 4% ratio molten
Wormwood essential oil and dispersing agent is added in deionized water in solution, stirs 40min, revolving speed 2000r/min, adjusts PH with 10% acetic acid
To 4,30min, revolving speed 2000r/min are stirred with magnetic stirrer, system is cooled to 1 DEG C, and be added under the low temperature environment
10% sodium hydroxide solution is 10 to PH, after blender stirring rate 2000r/min, mixing time 20min, replys room temperature and is added
25% glutaraldehyde stirs 3 hours and tannic acid stirs 4 hours, and it is 12 hours dry that drying machine is put into after stirring.
Then it carries out fibroin albumen doughnut 1 to prepare: by useless silk by 2:20's in the sodium carbonate liquor of 500g/l
Ratio bath raio boils 30min, is repeated 3 times, and fibroin is cleaned with 60 DEG C of deionized water after degumming, is then dried with baking oven.
The potassium bromide for being 41:59 with mass ratio and dehydrated alcohol are mixed into solvent at 80 DEG C, dissolve fibroin, at room temperature dipping expansion
8 hours.Fibroin albumen spinning solution is made, spinning solution is added in doughnut preparation facilities, it is hollow that silk fibroin is made
Fiber 1.
Wormwood microcapsules 2 are inserted later in the cavity of fibroin albumen doughnut 1: wormwood essential oil microcapsules are pressed 10%
Ratio, which is dispersed in water, is made dispersion, dispersion liquid is immersed in 1 one end of silk fibroin hollow fiber, other end access is opened
The rubber tube of mouth, the rubber tube other end connect vacuum pump, and vacuum pump is evacuated to fiber upper end and liquid occurs, vacuum pump closes
It closes.The doughnut freeze-drying that dispersion liquid will be filled, remove the moisture in dispersion liquid, and wormwood essential oil microcapsules are deposited in
In hollow fiber chamber.
The fibroin albumen doughnut of the microcapsules prepared by the above method containing wormwood, reaches and slows down in wormwood microcapsules 2
The volatilization of wormwood essential oil, and under normal temperature and pressure environment, wormwood essential oil volatilizees duration not 48 hours, i.e., using micro- containing wormwood
At the fibroin albumen doughnut of capsule 48 hours, remain to smell the distinctive fragrance of wormwood essential oil.
Comparative example: wormwood essential oil Direct Uniform is applied to Plastic film surface, observation wormwood essential oil volatilization situation is applying
After smearing wormwood essential oil 1 hour, wormwood essential oil can not be snuffed in the Plastic film surface for being coated with wormwood essential oil.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of fibroin albumen doughnut of microcapsules containing wormwood, which is characterized in that the fibroin albumen including being in hollow setting
Doughnut (1) is provided with several wormwood microcapsules (2) in the cavity of the fibroin albumen doughnut (1), and the wormwood is micro-
It is provided with wormwood essential oil in capsule (2), the wormwood microcapsules (2) are by gum arabic, gelatin, wormwood essential oil through complex coacervation
Freeze-drying is made afterwards.
2. a kind of fibroin albumen doughnut of microcapsules containing wormwood according to claim 1, which is characterized in that the Chinese mugwort
Careless microcapsules (2) partial size is 50~1200nm.
3. a kind of fibroin albumen doughnut of microcapsules containing wormwood according to claim 2, which is characterized in that the Chinese mugwort
Careless microcapsules (2) partial size is 100~500nm.
4. a kind of preparation method of the fibroin albumen doughnut of microcapsules containing wormwood, which comprises the steps of:
Step 1, gum arabic and Gelatin are added dropwise wormwood essential oil and are emulsified with dispersing agent in deionized water；
Step 2, the pH value that the solution after emulsification is adjusted to solution with acetum, reach PH=3-4, carry out multiple coacervation process,
Capsule material is set to be coated on essential oil surface；
Solution after step 3, multiple cohesion is cooled under 0 DEG C of environment through stirring in blender, is adjusted using sodium hydroxide solution,
Reach the PH=9-10 of solution, carries out low temperature alkalization；
The 25% glutaraldehyde stirring that volume ratio is 10ml/l is added after solution to be replied to room temperature in step 4, adds tannic acid and stirs
It mixes, wormwood microcapsules (2) powder is obtained after freeze-drying, wormwood microcapsules (2) are dispersed in water and mass fraction is made is
18%~22% dispersion liquid；
Silk is placed in sodium carbonate liquor and removes silk gum by step 5, obtains fibroin, then molten with potassium bromide/ethyl alcohol mixed solvent
Fibroin is solved, fibroin albumen spinning solution is obtained；
Spinning solution is spun into fibroin albumen doughnut (1) with hollow fiber spinning device by step 6, then fibroin albumen is hollow
Dispersion liquid is immersed in fiber (1) one end, and the rubber tube of other end access opening, rubber tube connects vacuum pump, true by vacuum pumping
There is liquid in sky to fibroin albumen doughnut (1) upper end, and vacuum pump is closed；
The doughnut for filling dispersion liquid is freeze-dried by step 7, the moisture in dispersion liquid is removed, by wormwood essential oil microcapsules
It is deposited in fibroin albumen doughnut (1) chamber.
5. a kind of preparation method of the fibroin albumen doughnut of microcapsules containing wormwood according to claim 4, feature
It is, in step 1, mass fraction is 3.8~4.2% to the gum arabic in deionized water, and gelatin mass fraction is 3.8
~4.2%, solution temperature is 40 DEG C, and wormwood essential oil mass fraction 11.8~12.2% stirs 30 minutes, and 10000 revs/min are stirred
20s is mixed, 3000~4000 revs/min, stirs 15 minutes, dispersing agent is then added while stirring.
6. a kind of preparation method of the fibroin albumen doughnut of microcapsules containing wormwood according to claim 4, feature
It is, in step 2, solution adjusts acetum used in PH, mass fraction 10%, stirring rate 3000- before agglomerating again
4000 revs/min, the reaction time is 30 minutes.
7. a kind of preparation method of the fibroin albumen doughnut of microcapsules containing wormwood according to claim 4, feature
Be, in step 3, solution is gradually cooled to 0~5 DEG C after multiple cohesion, temperature reach after with 10% sodium hydroxide solution adjusting PH
For 9-10, temperature is kept for 5 DEG C hereinafter, speed of agitator is 2000-3000 revs/min, and mixing time is 20 minutes.
8. a kind of preparation method of the fibroin albumen doughnut of microcapsules containing wormwood according to claim 4, feature
It is, in step 4,25% glutaraldehyde volume ratio is 10ml/l, and mixing time is 30 minutes；It moves on in 40 DEG C of thermostat water baths,
Mixing time 3h；Adding tannic acid usage ratio is 10g/l, mixing time 4.5h, is in revolving speed by the system after solidification
10min is centrifuged under the conditions of 5000 revs/min, freeze-drying obtains wormwood microcapsules (2) powder.
9. a kind of preparation method of the fibroin albumen doughnut of microcapsules containing wormwood according to claim 4, feature
It is, in step 5, silk boils 30min in the ratio bath raio of 1:20 in the sodium carbonate liquor of 500g/l, it is repeated 3 times,
Fibroin is cleaned with 60 DEG C of deionized water after degumming, is then dried with baking oven, the potassium bromide and anhydrous second for being 42:58 with mass ratio
Alcohol is mixed into solvent at 80 DEG C, dissolves fibroin, at room temperature dipping expansion 6-8 hours.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811268535.1A CN109183173B (en) | 2018-10-29 | 2018-10-29 | Silk fibroin hollow fiber containing wormwood microcapsule and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811268535.1A CN109183173B (en) | 2018-10-29 | 2018-10-29 | Silk fibroin hollow fiber containing wormwood microcapsule and preparation method thereof |
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| CN109183173A true CN109183173A (en) | 2019-01-11 |
| CN109183173B CN109183173B (en) | 2021-04-06 |
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| CN110359286A (en) * | 2019-07-12 | 2019-10-22 | 武汉纺织大学 | A kind of doughnut durability water-repellent finishing method |
| CN111701545A (en) * | 2020-06-04 | 2020-09-25 | 上海工程技术大学 | Dripping pill production system suitable for producing microcapsule formula soil conditioner |
| CN113774670A (en) * | 2021-08-20 | 2021-12-10 | 南通帝沙纺织有限公司 | Preparation method of antibacterial warm-keeping fabric |
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| CN109183173B (en) | 2021-04-06 |
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