CN106433151A - Antibacterial microcapsule with clove oil embedded in laurinol modified alginic acid derivative and preparation method of antibacterial microcapsule - Google Patents
Antibacterial microcapsule with clove oil embedded in laurinol modified alginic acid derivative and preparation method of antibacterial microcapsule Download PDFInfo
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- lauryl alcohol
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0084—Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
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- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
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Abstract
The invention relates to an antibacterial microcapsule with clove oil embedded in a laurinol modified alginic acid derivative and a preparation method of the antibacterial microcapsule, and belongs to the technical field of modification of high polymer materials. The antibacterial microcapsule comprises sodium alginate, laurinol and clove oil.The preparation method comprises the following steps that firstly laurinol is used to modify sodium alginate to obtain sodium alginate graft-copolymerized laurinol SA-Da, and then the clove oil is embedded to obtain the antibacterial microcapsule with the clove oil embedded in the laurinol modified alginic acid derivative. The prepared slow-release antibacterial microcapsule is relatively high in antibacterial property, can effectively inhibit the growth and propagation of microorganisms, has a certain slow release effect, slowly releases the antibacterial ingredient of the clove oil along with the change of time, has an excellent slow-release antibacterial effect, and can be applied to a food packaging film to prolong the food shelf-life and improve the food quality, and therefore, the antibacterial microcapsule has an excellent market prospect.
Description
Technical field
The present invention relates to a kind of antibacterial microcapsule of lauryl alcohol modification alginic acid derivative embedding Oleum Caryophylli and its preparation side
Method, belongs to field of high polymer material modification.
Background technology
Sodium alginate is kind of a polyelectrolyte, has an effect with bivalent cation, is tightly combined sodium alginate molecule interchain, leads to
Cross sodium alginate to mix with antibiotic substance, mixed liquor is slowly added drop-wise to containing divalent calcium ions aqueous solution with certain speed
In, form the gel micro-ball containing antibiotic substance and substantial amounts of research is obtained, but be found from research that in sodium alginate molecule and contain
There is substantial amounts of-COONa and-OH, be a kind of hydrophilic extremely strong polysaccharide polymer, relatively low to the embedding rate of hydrophobic antimicrobial agent,
There is phenomenon of burst release at the release initial stage.Low in order to solve the problems, such as the embedding rate to hydrophobic antimicrobial agent, a large amount of scholars are to Sargassum
Sour sodium is modified research, wherein mainly includes to be blended with other materials or to sodium alginate chemical modification.Sodium alginate divides
Contain substantial amounts of-COONa in son, by protonating to which so as to containing certain-COOH in molecular weight reduction and molecule,
In the presence of catalyst system and catalyzing, the acid sodium of the low molecular weight seaweed containing-COOH can be with some alcohols materials (as cholesterol, poly- second
Glycol) there is esterification, new polymer is formed, new polymer has two that one end is one section of hydrophobic group of hydrophilic group
Close compound.Amphipathic compound can be self-assembly of nucleocapsid of the hydrophobic group for core hydrophilic group for shell in aqueous and tie
Structure.Using this characteristic, can be good at hydrophobicity antibiotic substance is gathered in the core of hydrophobic group, and then improve its embedding
Rate.
Cholesterol is a kind of alcohols material of cyclopentanoperhy drophenanthrene, water insoluble, with stronger hydrophobicity, in catalytic materials
With the compound containing-COOH group, esterification can occur in the presence of matter, obtain novel substance.Lauryl alcohol also referred to as 12
Alcohol, water insoluble, it is often applied to the alcohols material of detergent, surfactant etc..Oleum Caryophylli main component is eugenol, is
A kind of natural antibacterial agent with preferable anti-microbial property, but Oleum Caryophylli is volatile in external environment, quicker to light, temperature
Sense, and water solublity is extremely low, and these all hinder which to apply in antibiotic packaging material.
In industry, the report is modified by sodium alginate is seldom seen at present.The present invention is urged using EDC-HCl and DMAP
Change system, lauryl alcohol graft copolymerization alginic acid forms amphipathic graft copolymer, is simultaneously introduced Oleum Caryophylli and is embedded, enhances slow
The property released and stability under various circumstances.
Content of the invention
It is an object of the invention to overcoming above-mentioned weak point, a kind of lauryl alcohol modification alginic acid derivative embedding fourth is provided
Antibacterial microcapsule of Oleum sesami and preparation method thereof.
According to the technical scheme that the present invention is provided, a kind of antibacterial of lauryl alcohol modification alginic acid derivative embedding Oleum Caryophylli is micro-
Capsule, formula proportion is as follows by weight：1 part of sodium alginate, 4～6 parts of lauryl alcohol and 0.5～1 part of Oleum Caryophylli；Initially with
Lauryl alcohol is modified for sodium alginate, is obtained sodium alginate graft copolymerization lauryl alcohol SA-Da, subsequently Oleum Caryophylli is wrapped
Bury, obtain the clove oil microcapsules that lauryl alcohol modification alginic acid derivative embeds Oleum Caryophylli.
The sodium alginate is natural sea alginic acid sodium powder, and mesh number is 250～350 mesh.
The preparation method of the antibacterial microcapsule of the lauryl alcohol modification alginic acid derivative embedding Oleum Caryophylli, by weight
Step is as follows：
(1) preparation of lauryl alcohol modification alginic acid derivative SA-Da：
A, according to Methanamide：DMF volume ratio 9～10：9 configuration mixed solutions；Weigh 1g alginic acid
Sodium, is put in 30～50mL mixed solution, and is rapidly added 0.4～0.6g p-methyl benzenesulfonic acid, stirring 25～45min of acidifying；So
Add 0.3～0.5g EDC-HCl and 0.4～0.6g DMAP DMAP to stir afterwards, be eventually adding 4～6g month
Cinnamic alcohol, 50～60 DEG C of stirring in water bath react 20～30h；
B, step a gained is reacted after solution pour in the ethanol solution of 170～180mL, and Quick spin 10
～30min is precipitated thing, and centrifugal rotational speed is 4000～5000rpm；By precipitate at 0～0.1MPa, 30～40 DEG C vacuum
20～30h is dry, obtains dried object；
C, step b gained dried object is dissolved in 30～50mL deionized water, stirs complete to dissolving, add quality dense
Spend the NaHCO for 2%3Aqueous solution adjusts pH to neutrality；By gained neutral solution, at 0～0.1MPa, -10～-2 DEG C, vacuum is done
Dry 20～30h obtains sodium alginate graft copolymerization lauryl alcohol SA-Da；
(2) preparation of clove oil microcapsules：0.5～1g Oleum Caryophylli is dissolved in 5～10mL ethanol solution, is obtained
Mixed solution；Take step (1) and prepare gained lauryl alcohol modification alginic acid derivative SA-Da and be dissolved completely in 15～30mL deionization
In water, Oleum Caryophylli and dehydrated alcohol mixed solution is subsequently added, above-mentioned solution is sufficiently stirred for reacting 1～3h；Gained is mixed
Solution 20～30h of vacuum lyophilization under the conditions of 0～0.5MPa, -10～-2 DEG C, that is, obtain product lauryl alcohol modification alginic acid
The clove oil microcapsules of derivant embedding Oleum Caryophylli.
Beneficial effects of the present invention：The present invention is modified to sodium alginate using lauryl alcohol, improves sodium alginate hydrophilic
Property, parents' group is formed, improves the stability that sodium alginate embeds Oleum Caryophylli, it is to avoid phenomenon of burst release.
The present invention is under EDC-HCl and DMAP reaction system, and lauryl alcohol can occur chemistry with the derivant of sodium alginate
Reaction, sodium alginate molecular structure graft copolymerization hydrophobic group lauryl alcohol is formed has amphipathic new polymer (SA-Da).
Lauryl alcohol graft modification sodium alginate (SA-Da) can be self-assembly of nucleocapsid structure in aqueous solution, Oleum Caryophylli be had good
Inclusion, and embedding rate increases with the increase of the percent grafting of polymer.
Clove oil microcapsules prepared by the present invention have good stability, and have in high temperature environments good steady
Qualitative, prevent Oleum Caryophylli from quickly volatilizing in atmosphere.The source such as Oleum Caryophylli, sodium alginate, lauryl alcohol used in the present invention is wide
General and all nontoxic to human body.
The present invention prepare sustained-release antibacterial capsule have stronger anti-microbial property, effectively can suppress microorganism growth and
Breeding, and with certain slow release effect, change that can be over time, slow release Oleum Caryophylli antimicrobial component, with good
Sustained-release antibacterial effect, can operate with food package film, strengthen effective period of food quality, raising food quality, therefore good market prospects.
Description of the drawings
The infrared spectrogram of Fig. 1 lauryl alcohol modification alginic acid derivative SA-Da.
The volatility curve of Oleum Caryophylli and clove oil microcapsules in Fig. 2 24h；sa：Oleum Caryophylli；da：Lauryl alcohol and alginic acid
The graft copolymer embedding Oleum Caryophylli of sodium.
Preparation curve of Fig. 3 clove oil microcapsules in simulated solution；sa：Sodium alginate embeds Oleum Caryophylli；Da-
1：Lauryl alcohol is 4 with sodium alginate mass ratio:1 graft copolymer embeds Oleum Caryophylli；da-2：Lauryl alcohol and sodium alginate mass ratio
For 5:1 graft copolymer embeds Oleum Caryophylli；da-3：Lauryl alcohol is 6 with sodium alginate mass ratio:1 graft copolymer embeds Flos Caryophylli
Oil.
The antibacterial circle diameter of Fig. 4 clove oil microcapsules change curve over time；sa：Sodium alginate embeds Oleum Caryophylli；Da-
1：Lauryl alcohol is 4 with sodium alginate mass ratio:1 graft copolymer embeds Oleum Caryophylli；da-2：Lauryl alcohol and sodium alginate mass ratio
For 5:1 graft copolymer embeds Oleum Caryophylli；da-3：Lauryl alcohol is 6 with sodium alginate mass ratio:1 graft copolymer embeds Flos Caryophylli
Oil.
Specific embodiment
The present invention is further illustrated with reference to embodiments.
The comprehensive sustained-release antibacterial performance of material is determined by clove oil microcapsules anti-microbial property, Flos Caryophylli oil capsule is molten in simulation
The release test of release test and clove oil microcapsules of the release test, clove oil microcapsules in liquid in hermetic container is carried out
Judge.
In the present invention, instrument used mainly has：High speed agitator (IKA company), centrifuge (Shanghai), vacuum drying
Case, big dragon pipettor, FC104 electronic analytical balance (Shanghai precision scientific instrument company), magnetic stirring apparatuss (Jiangsu high honour instrument
Manufacturing Co., Ltd), UV-2000 type ultraviolet-visible light photometer (UNICO(Shanghai) Instruments Co., Ltd.), Nicolet
Nexus Fourier transform infrared spectroscopy (Thermo Electron Corporation), Portable pressure steam sterilizing pot (on
Hai Shenan medical apparatus and instruments factory), intelligent growth cabinet (Changzhou Nuo Ji Instrument Ltd.), single clean work station (Su Jingjing
Change equipment company limited), Desk type constant-temperatureoscillator oscillator (Changzhou Nuo Ji Instrument Ltd.), (fast industry is won in Shanghai to biochemical cultivation case
Medical Equipment Plant of company limited).
Embodiment 1
(1) preparation of lauryl alcohol modification alginic acid derivative SA-Da：
A, according to Methanamide：DMF volume ratio 10：9 configuration mixed solutions；1g sodium alginate is weighed, is put
Enter in 40mL mixed solution, and 0.5g p-methyl benzenesulfonic acid is rapidly added, stirring acidifying 35min；It is subsequently adding 0.4g EDC-HCl
Stir with 0.5g DMAP DMAP, 5g lauryl alcohol is eventually adding, 55 DEG C of stirring in water bath react 24h；
B, step a gained is reacted after solution pour in the ethanol solution of 175mL, and Quick spin 15min is obtained
To precipitate, centrifugal rotational speed is 5000rpm；Precipitate is vacuum dried 20h at 0～0.1MPa, 30～40 DEG C, obtains drying
Thing；
C, step b gained dried object is dissolved in 40mL deionized water, stirs complete to dissolving, add the mass concentration to be
2% NaHCO3Aqueous solution adjusts pH to neutrality；Gained neutral solution is vacuum dried at 0～0.1MPa, -10～-2 DEG C
25h obtains sodium alginate graft copolymerization lauryl alcohol SA-Da；
Characterize：Sample being prepared with pressed disc method, the spectrogram of SA-Da is determined on infrared spectrum, verifies the formation of copolymer,
Concrete as shown in Figure 1.
(2) preparation of clove oil microcapsules：The lauryl alcohol modification alginic acid derivative SA-Da that step (1) prepares gained is taken,
It is dissolved completely in 15mL deionized water, blank micella is prepared into, is subsequently added and weighs 0.6g Oleum Caryophylli and be dissolved completely in
5mL ethanol solution, both are thoroughly mixed 2 hours, 0～0.5MPa, vacuum lyophilization under the conditions of -10～-2 DEG C
25h, obtains the clove oil microcapsules that lauryl alcohol modification alginic acid derivative embeds Oleum Caryophylli.
(3) test result：Sodium alginate is 24.86% to the embedding rate of Oleum Caryophylli；Under 100 DEG C of hot environments, Flos Caryophylli
The volatility 14.11% of oil microcapsule；In hermetic container, clove oil microcapsules were at first 4 days, and rate of release is very fast, cumulative release
Rate is 20.12%, and As time goes on, at 4 to 28 days, its rate of release slows down, the rate of release for keeing relative stability, 28
After it, cumulative release speed is 60.02%；In simulated solution, clove oil microcapsules accumulation volatility in 200h is
72.09%；Its antibacterial circle diameter area is 33.39mm2.
Embodiment 2
(1) preparation of lauryl alcohol modification alginic acid derivative SA-Da：
A, according to Methanamide：DMF volume ratio 9：9 configuration mixed solutions；1g sodium alginate is weighed, is put
Enter in 30mL mixed solution, and 0.4g p-methyl benzenesulfonic acid is rapidly added, stirring acidifying 25min；It is subsequently adding 0.3g EDC-HCl
Stir with 0.4g DMAP DMAP, 4g lauryl alcohol is eventually adding, 50 DEG C of stirring in water bath react 30h；
B, step a gained is reacted after solution pour in the ethanol solution of 170mL, and Quick spin 30min is obtained
To precipitate, centrifugal rotational speed is 4000rpm；Precipitate is vacuum dried 30h at 0～0.1MPa, 30～40 DEG C, obtains drying
Thing；
C, step b gained dried object is dissolved in 30mL deionized water, stirs complete to dissolving, add the mass concentration to be
2% NaHCO3Aqueous solution adjusts pH to neutrality；Gained neutral solution is vacuum dried at 0～0.1MPa, -10～-2 DEG C
30h obtains sodium alginate graft copolymerization lauryl alcohol SA-Da；
(2) preparation of clove oil microcapsules：Sodium alginate graft copolymerization lauryl alcohol SA-Da obtained in step (1) is taken, completely
It is dissolved in 30mL deionized water, blank micella is prepared into, is subsequently added and weighs 0.8g Oleum Caryophylli and be dissolved completely in 10mL
Ethanol solution, both are thoroughly mixed 2 hours, 0～0.5MPa, vacuum lyophilization under the conditions of -10～-2 DEG C
20h, obtains the clove oil microcapsules that lauryl alcohol modification alginic acid derivative embeds Oleum Caryophylli.
(3) test result：Sodium alginate is 35.28% to the embedding rate of Oleum Caryophylli；Under 100 DEG C of hot environments, Flos Caryophylli
The volatility 14.11% of oil microcapsule；In hermetic container, clove oil microcapsules were at first 4 days, and rate of release is very fast, cumulative release
Rate is 19.37%, and As time goes on, at 4 to 28 days, its rate of release slows down, the rate of release for keeing relative stability, 28
After it, cumulative release speed is 51.52%；In simulated solution, clove oil microcapsules accumulation volatility in 200h is
57.31%；Its antibacterial circle diameter area is 20.52mm2.
Embodiment 3
(1) preparation of lauryl alcohol modification alginic acid derivative SA-Da：
A, according to Methanamide：DMF volume ratio 10：9 configuration mixed solutions；1g sodium alginate is weighed, is put
Enter in 40mL mixed solution, and 0.6g p-methyl benzenesulfonic acid is rapidly added, stirring acidifying 45min；It is subsequently adding 0.5g EDC-HCl
Stir with 0.6g DMAP DMAP, 6g lauryl alcohol is eventually adding, 60 DEG C of stirring in water bath react 20h；
B, step a gained is reacted after solution pour in the ethanol solution of 170mL, and Quick spin 20min is obtained
To precipitate, centrifugal rotational speed is 4500rpm；Precipitate is vacuum dried 25h at 0～0.1MPa, 30～40 DEG C, obtains drying
Thing；
C, step b gained dried object is dissolved in 50mL deionized water, stirs complete to dissolving, add the mass concentration to be
2% NaHCO3Aqueous solution adjusts pH to neutrality；Gained neutral solution is vacuum dried at 0～0.1MPa, -10～-2 DEG C
25h obtains sodium alginate graft copolymerization lauryl alcohol SA-Da；
(2) preparation of clove oil microcapsules：Lauryl alcohol modification alginic acid derivative SA-Da obtained in step (1) is taken, completely
Be dissolved in 25mL deionized water, be prepared into blank micella, be subsequently added be completely dissolved 1g Oleum Caryophylli 5mL dehydrated alcohol molten
Liquid, both are thoroughly mixed 2 hours, 0～0.5MPa, vacuum lyophilization 25h under the conditions of -10～-2 DEG C, obtain Laurel
Alcohol modification alginic acid derivative embeds the clove oil microcapsules of Oleum Caryophylli.
(3) test result：Sodium alginate is 35.10% to the embedding rate of Oleum Caryophylli；Under 100 DEG C of hot environments, Flos Caryophylli
The volatility 14.11% of oil microcapsule；In hermetic container, clove oil microcapsules were at first 4 days, and rate of release is very fast, cumulative release
Rate is 20.15%, and As time goes on, at 4 to 28 days, its rate of release slows down, the rate of release for keeing relative stability, 28
After it, cumulative release speed is 54.81%；In simulated solution, clove oil microcapsules accumulation volatility in 200h is
59.36%；Its antibacterial circle diameter area is 19.45mm2.
Application Example 1
(1) percent grafting to sodium alginate graft copolymerization lauryl alcohol SA-Da and the embedding rate of clove oil microcapsules are surveyed
Examination, concrete test result is as shown in table 1.
Table 1
As shown in Table 1, alginic acid is 1 with the mass ratio of lauryl alcohol:4, its percent grafting reaches 12.15%, in mass ratio is
1:5, its percent grafting is reached for 20.30%, and with the increase of the quality of lauryl alcohol, becoming of reducing afterwards occurs first increasing in percent grafting
Gesture, when mass ratio is 1:5 reach maximum.Sodium alginate to the embedding rate of Oleum Caryophylli be 10.25%, its modified Da-1, Da-2,
Da-3 respectively reaches 24.86%, 35.28%, 35.10%, is obviously improved.With the lifting of percent grafting, in polymer
Hydrophobic group Laurel alcohol radical be continuously increased, its hydrophobic performance is improved, and embedding rate constantly increases, in the embedding of Oleum Caryophylli
It is obviously improved in effect.
(2) clove oil microcapsules for preparing gained using embodiment are simulated waving in solution (i.e. ethanol solution)
Test is sent out, in 24h, Oleum Caryophylli is as shown in Figure 2 with the volatility curve of clove oil microcapsules；
As shown in Figure 2, unmodified sodium alginate directly embeds Oleum Caryophylli and kept rate of release faster at first 20 days, and 25 arrive
In 28 days, its rate of release slows down, and the Oleum Caryophylli of embedding is almost depleted, and preparation reaches 88%；Modified Sargassum
Sour sodium embedding Oleum Caryophylli forms microcapsule, and its sustained release performance gets a promotion, and at first 4 days, rate of release was very fast, and preparation divides
Not Wei 20.12%, 19.37%, 20.15%, be almost consistent with unmodified sodium alginate, this is that have due to the surface of sample
The Oleum Caryophylli of residual causes, and As time goes on, at 4 to 28 days, its rate of release slows down, the release speed for keeing relative stability
Rate, after 28 days cumulative release speed be respectively 60.02%, 51.52%, 54.81%, with unmodified sample formed significantly poor
Different.Its release process trend of the clove oil microcapsules of different percent graftings is consistent, rate of release da-1 of Oleum Caryophylli>Da-2,
Da-3 and da-2 almost keeps phase same rate and trend, and with the raising of percent grafting, its rate of release also slows down accordingly.Cause
And, the microcapsule of lauryl alcohol modified sodium alginate embedding Oleum Caryophylli formation, can continue in atmosphere slowly to discharge Oleum Caryophylli,
With certain sustained release performance.
(3) clove oil microcapsules for preparing gained using embodiment are simulated carrying out in solution (i.e. ethanol solution)
Preparation is tested, and concrete release rate curve chart is as shown in Figure 3；
From the figure 3, it may be seen that at first 4 hours, four samples all quickly discharged Oleum Caryophylli, unmodified sodium alginate release speed
Rate is far longer than the clove oil microcapsules of modified preparation, unmodified sodium alginate after 2 hours preparation reach
73.1%, illustrating that sodium alginate soln is mixed with Oleum Caryophylli can not embed to Oleum Caryophylli, and substantial amounts of Oleum Caryophylli is attached to Sargassum
Sour sodium surface.
Release rate curve of the microcapsule that different percent graftings are formed in simulated solution keeps identical trend, and the initial stage is a large amount of
Release, when the Oleum Caryophylli of surface of microcapsule is released, release process tends to slowly and steadily discharge, in 200h, Da-1,
The preparation of Da-2, Da-3 is respectively 72.09%, 57.31%, 59.36, its cumulative release speed da-1>Da-2, da-3
Phase same rate and trend are almost kept with da-2, with the lifting of percent grafting, the increase of hydrophobic group, the micro- glue of the Oleum Caryophylli of formation
Capsule can be more stable slowly discharge in simulated solution, sustained release performance obtains certain lifting.
(4) clove oil microcapsules for preparing gained using embodiment carry out antibacterial circle diameter test, the micro- glue of concrete Oleum Caryophylli
Change curve is as shown in Figure 4 over time for the antibacterial circle diameter of capsule；
As shown in Figure 4, due to there is a small amount of Oleum Caryophylli to be attached to surface of microcapsule, just started to keep preferable fungistatic effect,
But the volatilization with surface Oleum Caryophylli, the fungistatic effect of clove oil microcapsules is gradually reduced, at the 6th day, unmodified alginic acid
The inhibition zone area 33.41mm of sodium embedding Oleum Caryophylli2, continuation holding downward trend, different percent grafting clove oil microcapsules da-1,
Da-2, da-3 antibacterial circle diameter area be 33.39,20.52,19.45mm2, subsequently keep stable fungistatic effect.Sodium alginate
The microcapsule that grafted hydrophobic group is formed can effectively hinder dissolution or the diffusion of Oleum Caryophylli, continue slowly in the later stage so as to which
Release Oleum Caryophylli.
The above-mentioned description to embodiment is to be understood that for ease of those skilled in the art and apply this
Bright.Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein
General Principle is applied to without through performing creative labour in other embodiment.Therefore, the invention is not restricted to enforcement here
Example, those skilled in the art are according to the announcement of the present invention, and the improvement that is made without departing from scope and modification all should be
Within protection scope of the present invention.
Claims (3)
1. a kind of lauryl alcohol modification alginic acid derivative embeds the antibacterial microcapsule of Oleum Caryophylli, it is characterized in that formula proportion by weight
Part meter is as follows：1 part of sodium alginate, 4 ~ 6 parts of lauryl alcohol and 0.5 ~ 1 part of Oleum Caryophylli；Enter for sodium alginate initially with lauryl alcohol
Row is modified, obtains sodium alginate graft copolymerization lauryl alcohol SA-Da, subsequently Oleum Caryophylli is embedded, and obtains the modified sea of lauryl alcohol
The clove oil microcapsules of alginate derivatives embedding Oleum Caryophylli.
2. antibacterial microcapsule as claimed in claim 1, is characterized in that：The sodium alginate is natural sea alginic acid sodium powder, and mesh number is
250 ~ 350 mesh.
3. described in claim 1, lauryl alcohol modification alginic acid derivative embeds the preparation method of the antibacterial microcapsule of Oleum Caryophylli, its
It is characterized in that step is as follows by weight：
（1）The preparation of lauryl alcohol modification alginic acid derivative SA-Da：
A, according to Methanamide：DMF volume ratio 9 ~ 10：9 configuration mixed solutions；1g sodium alginate is weighed, is put into
In 30 ~ 50mL mixed solution, and 0.4 ~ 0.6g p-methyl benzenesulfonic acid is rapidly added, stirring 25 ~ 45min of acidifying；It is subsequently adding 0.3 ~
0.5g EDC-HCl and 0.4 ~ 0.6g DMAP DMAP stir, and are eventually adding 4 ~ 6g lauryl alcohol, 50 ~ 60 DEG C
Stirring in water bath reacts 20 ~ 30h；
B, step a gained is reacted after solution pour in the ethanol solution of 170 ~ 180mL, and 10 ~ 30min of Quick spin
Thing is precipitated, centrifugal rotational speed is 4000 ~ 5000rpm；Precipitate is vacuum dried 20 ~ 30h at 0 ~ 0.1MPa, 30 ~ 40 DEG C,
Obtain dried object；
C, step b gained dried object is dissolved in 30 ~ 50mL deionized water, stirs complete to dissolving, add the mass concentration to be
2% NaHCO3Aqueous solution adjusts pH to neutrality；Gained neutral solution is vacuum dried at 0 ~ 0.1MPa, -10 ~ -2 DEG C 20 ~
30h obtains sodium alginate graft copolymerization lauryl alcohol SA-Da；
（2）The preparation of clove oil microcapsules：0.5 ~ 1g Oleum Caryophylli is dissolved in 5 ~ 10mL ethanol solution, obtains mixing molten
Liquid；Take step（1）Prepare gained lauryl alcohol modification alginic acid derivative SA-Da to be dissolved completely in 15 ~ 30mL deionized water, with
Add Oleum Caryophylli and dehydrated alcohol mixed solution afterwards, above-mentioned solution is sufficiently stirred for reacting 1 ~ 3h；By gained mixed solution 0 ~
0.5MPa, 20 ~ 30h of vacuum lyophilization under the conditions of -10 ~ -2 DEG C, that is, obtain the modification alginic acid derivative embedding of product lauryl alcohol
The clove oil microcapsules of Oleum Caryophylli.
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| CN107325545A (en) * | 2017-08-28 | 2017-11-07 | 安徽智博新材料科技有限公司 | One kind sustained release medicine-chest filled type slow-release material |
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| CN114644763B (en) * | 2022-03-21 | 2024-05-28 | 江南大学 | Pickering emulsion with clove oil embedded in amphiphilic thermal gel and preparation method thereof |
| CN114921865A (en) * | 2022-05-31 | 2022-08-19 | 邦特云纤(青岛)新材料科技有限公司 | Regenerated cellulose fiber containing avocado and shea butter extract nanoparticles and preparation method thereof |
| CN114921865B (en) * | 2022-05-31 | 2024-04-05 | 邦特云纤(青岛)新材料科技有限公司 | Regenerated cellulose fiber containing nanometer particles of extracts of avocado and shea and preparation method thereof |
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