CN106750382B - A kind of preparation method of chitosan gel rubber pearl - Google Patents
A kind of preparation method of chitosan gel rubber pearl Download PDFInfo
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- CN106750382B CN106750382B CN201611176504.4A CN201611176504A CN106750382B CN 106750382 B CN106750382 B CN 106750382B CN 201611176504 A CN201611176504 A CN 201611176504A CN 106750382 B CN106750382 B CN 106750382B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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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
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
Abstract
The invention discloses a kind of capsule shape and can contain small molecule dyes chitosan gel rubber pearl preparation method, belong to chitosan gel rubber pearl fabricating technology field.It is somebody's turn to do the preparation method comprises the following steps: chitosan is dissolved in acetum, and sodium β-glycerophosphate pentahydrate solution is slowly added dropwise in ice-water bath.And mixed solution pH value is adjusted to neutrality.Prepared chitosan/sodium β-glycerophosphate pentahydrate mixed solution (CS/ β-GP solution) is instilled in SDS receiving liquid, forms the chitosan drop of package CS/ β-GP solution after curing.After heating water bath, gelation occurs for the internal effect due to hydrogen bond, finally obtains chitosan gel rubber pearl.Chitosan gel rubber pearl prepared by the present invention has excellent containing property to small molecule dyes of the molecular weight between 300-800, and dye leakage amount is few, and it is good to contain stability, still without obvious leakage after 12h.
Description
Technical field
The invention belongs to chitosan gel rubber pearl preparation process field, especially a kind of capsule shape and small molecule dyes can be contained
Chitosan gel rubber pearl preparation method.
Technical background
Chitosan (chitosan, CS) is white or canescence, slightly has pearly luster, translucent chip solid, also known as de-
Acetyl chitin, soluble chitin, poly glucosamine are the products of chitin deacetylation.The average molecular of chitosan
Quality is differed from hundreds of thousands of to millions of, and molecular formula is (C6HllO4N) n, monomer are mostly 2- amino-D-Glucose.Chitosan
Solubility property is better than chitin, dissolves in dilute organic acid and part inorganic acid, such as lactic acid, hydrochloric acid and acetic acid, but do not dissolve in
The chitosan of dilute sulfuric acid, dust technology, phosphoric acid,diluted, oxalic acid, not soluble in water and aqueous slkali, low viscosity can even be dissolved in water.
N- deacetylation and viscosity (can reflect average molecular mass) are two main character indexs of chitosan.One
As for, deacetylation (deacetylation degree, DD) is referred to as chitosan in 50% or more chitin, deacetylated
Degree is higher, and the amino rate of ionization in chitosan molecule chain is higher, more soluble easily in water.It, can be according to the difference of viscosity
Chitosan is divided into three kinds.The 1% chitosan acetic acid solution usually viscosity in 1000cps or more calls high-viscosity chitosan, glues
It spends and is known as medium viscosity chitosan in 100~1000cps, be sticked to 100cps referred to as low viscosity chitosan below.Other conditions
In identical situation, the viscosity of chitosan is bigger, and solubility in water is smaller.
Chitosan-sodium glycero-phosphate thermo-sensitive gel system is seen 2000 earliest, once proposition, that is, is paid high attention to.
It is that the system uses natural macromolecular material chitosan first, biocompatibility is gradually ground with biodegradability
The approval for the person of studying carefully.In addition, simple chitosan only keeps solution state under acidic environment, when pH value is increased to 6.9-7.1,
Chitosan solution starts to precipitate, but in the presence of weak base sodium glycero-phosphate, which can keep in neutral conditions stable
Solution state, this provides convenience condition for the protein-based drug of system loads cell even living.It is finally that this is
System has temperature-sensing property, is in solution state below room temperature, and temperature is increased to curable formation gel when body temperature, so as to slow
Release the effect of load drug.If but being loaded directly into protein-based drug with chitosan-sodium glycero-phosphate thermo-sensitive gel system
Even cell living still remains some problems:
1. the form of gel is uncertain.
2. containing the small molecules such as the drug dyestuff inside gel may in transmittance process due to the unclosed property of gel
Gel can be detached from.
3. it is very poor that individual gel contains drug mechanical strength, contains structure and be easy to be destroyed.
For above some problems, the present invention develops a kind of with closure and the certain capsule shape gel beads of form.
Summary of the invention
The technical problems to be solved by the present invention are: provide a kind of capsule shape and can contain small molecule dyes chitosan it is solidifying
The preparation method of glue bead.It is designed by the structure of microcapsule coated microgel, Lai Tigao dyestuff contains stability, reduces leakage
Amount.
The present invention solves its technical problem, and the following technical solution is employed:
The preparation method of chitosan gel rubber pearl provided by the invention, specifically: first by chitosan and sodium β-glycerophosphate
Mixed solution by liquid-transfering gun, be added drop-wise in anionic surfactant solution, be based on chitosan and anion surface active
The cohesion of agent, forming core material, there are also the chitosan capsules of chitosan and sodium β-glycerophosphate；Then, by heating, make glue
The chitosan and sodium β-glycerophosphate in intracapsular portion form gel, finally obtain chitosan gel rubber pearl by hydrogen bond action.
The preparation method of the chitosan gel rubber pearl, comprising the following steps:
(1) chitosan/sodium β-glycerophosphate pentahydrate mixed solution preparation:
1.2g-1.6g sodium β-glycerophosphate pentahydrate is dissolved in 2mL water, and the medium viscosity chitosan of 0.4g is molten
Solution is in the acetum of 0.1mol/L；Under ice-water bath, β-phosphoglycerol is slowly added dropwise into the chitosan solution dissolved
Sodium pentahydrate solution obtains chitosan/sodium β-glycerophosphate pentahydrate mixed solution, and it is molten to be referred to as CS/ β-GP mixing
Liquid；
(2) adjusting of chitosan/sodium β-glycerophosphate pentahydrate mixed solution pH value and sodium dodecyl sulfate solution
Preparation:
It weighs 25g disodium hydrogen phosphate solid to be dissolved in 100ml water, dissolves the disodium phosphate soln being saturated；To CS/
The disodium phosphate soln of β-GP mixed solution and dripping saturation adjusts pH value between 6.9-7.1；Weigh 0.2g-0.8 12
Sodium alkyl sulfate solid is dissolved in 20mL water, is prepared the lauryl sodium sulfate receiving liquid of mass fraction 1%-4%, is referred to as
SDS receiving liquid；
(3) preparation of chitosan gel rubber pearl:
It is instilled in SDS receiving liquid with liquid-transfering gun by the CS/ β-GP solution that pH value is 6.9-7.1 is regulated, is obtained after curing
Then chitosan microcapsules are washed with distilled water 3 times, place into water-bath and heat, the CS/ β-GP solution inside microcapsules turns
Become gel, to obtain chitosan gel rubber pearl.
In the above method, the medium viscosity chitosan, viscosity is 200-400mPa.s, deacetylation >=90%.
In the above method, CS/ β-GP solution can be instilled in SDS receiving liquid, curing time 50-70min.
In the above method, the pH value that weakly alkaline solution adjusts CS/ β-GP solution can be used, which uses phosphorus
Sour disodium hydrogen or potassium dihydrogen phosphate.
In the above method, when chitosan microcapsules are changed into gel beads, bath temperature is 39-45 DEG C, water bath time 4-
7min。
In the above method, the mass ratio of chitosan and sodium β-glycerophosphate is 1/3-1/4.
The chitosan gel rubber pearl of above method preparation provided by the invention, is containing the application in small molecule dyes.
The chitosan gel rubber pearl is in application, it has excellent contain to small molecule dyes of the molecular weight between 350-800
Property, 12 hours are placed without obvious leakage, contain stability with good.
The present invention have compared with prior art it is following main the utility model has the advantages that
1. CS/GP mixed solution directly can be instilled in SDS acceptable solution and obtain gel beads in heating water bath, internal gel with
External clad structure one-pass molding is not necessarily to following process, reduces manufacture difficulty, improves producing efficiency.
2. the chitosan gel rubber ball being prepared can be applied to the cladding of small molecule dyes.The molecular weight for containing dyestuff exists
Between 300-800, dye leakage amount is few, and it is good to contain stability, still without obvious leakage after 12h.
3. the gel beads being prepared all have the excellent effect that contains to a variety of dyestuffs, such as to fluorescein sodium (molecule
Amount for 376), rhodamine B (molecular weight 479), Congo red (molecular weight 697) etc. have preferable package effect.
4. the gel beads being prepared can be observed more intuitively due to the high transparency of its own and be contained dye inside gel beads
Expect the leak case of dyestuff, it will not be due to the Color influences observing effect of gel beads itself.Such as preparation is contained into fluorescence
The gel beads of plain sodium dyestuff are immersed in the aqueous solution of 50ml, are stood overnight at room temperature, and research is coated in gel ball
The leak case of the fluorescein sodium in portion.As shown in Figure 1, the chitosan gel rubber pearl after temperature-induced gelation, has fluorescein sodium
There is preferable covered effect, and effectively reduces the leakage of fluorescein sodium in aqueous solution in chitosan gel rubber pearl.
Detailed description of the invention
Fig. 1 is the inside SEM figure of chitosan microcapsules.
Fig. 2 is the inside SEM figure of temperature-induced rear chitosan/sodium glycero-phosphate composite micro-capsule.
Fig. 3 is to have coated the chitosan gel rubber pearl of fluorescein sodium to place the shape appearance figure of 12h in water.
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described, and certain following embodiments should not be construed as pair
Limitation of the invention.
1. a kind of preparation method of the chitosan gel rubber pearl of capsule shape:
Embodiment 1:
1.4g sodium β-glycerophosphate pentahydrate is dissolved in 2mL water, and is 200-400mPa.s's by 0.4g viscosity
Medium viscosity chitosan is dissolved in the acetum of 0.1mol/L.Stirring is accelerated to dissolve it quickly.Standing after dissolution keeps shell poly-
Bubble in sugar juice sheds completely.It weighs 25g disodium hydrogen phosphate solid to be dissolved in 100ml water, the phosphoric acid hydrogen two being saturated
Sodium solution.Under ice-water bath, sodium β-glycerophosphate pentahydrate solution is slowly added dropwise into the chitosan solution dissolved, is added dropwise
After the completion, pH value is adjusted with the disodium phosphate soln of saturation to mix to chitosan/sodium β-glycerophosphate between 6.9-7.1, is obtained
It closes solution (CS/ β-GP mixed solution).It weighs 0.2g-0.8g lauryl sodium sulfate solid to be dissolved in 20mL water, prepares quality
The sodium dodecyl sulfate solution of score 2% is as receiving liquid.CS/ β-GP mixed solution is instilled in receiving liquid with liquid-transfering gun,
Curing can form translucent white globules in 1 hour.It is washed with distilled water bead 3 times, places into 42 DEG C of water-baths and keep the temperature
The chitosan gel rubber pearl of capsule shape can be obtained in 5min.
Embodiment 2:
It is formulated according to embodiment 1, the change curing time is 50min, and condition is constant.It is prepared according to the step of embodiment 1
The chitosan gel rubber pearl for the capsule shape that present case is implemented.The dosage of sodium β-glycerophosphate pentahydrate is 1.4g, and medium viscosity shell is poly-
The dosage of sugar is 0.4g, acetate concentration 0.1mol/L, adjusts pH value between 6.9-7.1, lauryl sodium sulfate dosage is
0.2g, bath temperature are 42 DEG C, water bath time 5min.Also the excellent chitosan gel rubber pearl of gel effect can be obtained.
Embodiment 3:
It is formulated according to embodiment 1, the change curing time is 60min, and condition is constant.It is prepared according to the step of embodiment 1
The chitosan gel rubber pearl for the capsule shape that present case is implemented.The dosage of sodium β-glycerophosphate pentahydrate is 1.4g, and medium viscosity shell is poly-
The dosage of sugar is 0.4g, acetate concentration 0.1mol/L, adjusts pH value between 6.9-7.1, lauryl sodium sulfate dosage is
0.2g, bath temperature are 42 DEG C, water bath time 5min.Also the excellent chitosan gel rubber pearl of gel effect can be obtained.
Embodiment 4:
It is formulated according to embodiment 1, the change curing time is 70min, and condition is constant.It is prepared according to the step of embodiment 1
The chitosan gel rubber pearl for the capsule shape that present case is implemented.The dosage of sodium β-glycerophosphate pentahydrate is 1.4g, and medium viscosity shell is poly-
The dosage of sugar is 0.4g, acetate concentration 0.1mol/L, adjusts pH value between 6.9-7.1, lauryl sodium sulfate dosage is
0.2g, bath temperature are 42 DEG C, water bath time 5min.Also the excellent chitosan gel rubber pearl of gel effect can be obtained.
Embodiment 5:
It is formulated according to embodiment 1, bath temperature is changed to 39 DEG C, and condition is constant.This case is prepared according to the step of embodiment 1
The chitosan gel rubber pearl for the capsule shape that example is implemented.The dosage of sodium β-glycerophosphate pentahydrate is 1.4g, medium viscosity chitosan
Dosage is 0.4g, acetate concentration 0.1mol/L, adjusts pH value between 6.9-7.1, and lauryl sodium sulfate dosage is 0.2g,
Curing time is 1h, water bath time 5min.Also the excellent chitosan gel rubber pearl of gel effect can be obtained.
Embodiment 6:
It is formulated according to embodiment 1, bath temperature is changed to 42 DEG C, and condition is constant.This case is prepared according to the step of embodiment 1
The chitosan gel rubber pearl for the capsule shape that example is implemented.The dosage of sodium β-glycerophosphate pentahydrate is 1.4g, medium viscosity chitosan
Dosage is 0.4g, acetate concentration 0.1mol/L, adjusts pH value between 6.9-7.1, and lauryl sodium sulfate dosage is 0.2g,
Curing time is 1h, water bath time 5min.Also the excellent chitosan gel rubber pearl of gel effect can be obtained.
Embodiment 7:
It is formulated according to embodiment 1, bath temperature is changed to 45 DEG C, and condition is constant.This case is prepared according to the step of embodiment 1
The chitosan gel rubber pearl for the capsule shape that example is implemented.The dosage of sodium β-glycerophosphate pentahydrate is 1.4g, medium viscosity chitosan
Dosage is 0.4g, acetate concentration 0.1mol/L, adjusts pH value between 6.9-7.1, and lauryl sodium sulfate dosage is 0.2g,
Curing time is 1h, water bath time 5min.Also the excellent chitosan gel rubber pearl of gel effect can be obtained.
Embodiment 8:
It is formulated according to embodiment 1, water bath time is changed to 4min, and condition is constant.This case is prepared according to the step of embodiment 1
The chitosan gel rubber pearl for the capsule shape that example is implemented.The dosage of sodium β-glycerophosphate pentahydrate is 1.4g, medium viscosity chitosan
Dosage is 0.4g, acetate concentration 0.1mol/L, adjusts pH value between 6.9-7.1, and lauryl sodium sulfate dosage is 0.2g,
Curing time is 1h, and bath temperature is 42 DEG C.Also the excellent chitosan gel rubber pearl of gel effect can be obtained.
Embodiment 9:
It is formulated according to embodiment 1, water bath time is changed to 7min, and condition is constant.This case is prepared according to the step of embodiment 1
The chitosan gel rubber pearl for the capsule shape that example is implemented.The dosage of sodium β-glycerophosphate pentahydrate is 1.4g, medium viscosity chitosan
Dosage is 0.4g, acetate concentration 0.1mol/L, adjusts pH value between 6.9-7.1, and lauryl sodium sulfate dosage is 0.2g,
Curing time is 1h, and bath temperature is 42 DEG C.Also the excellent chitosan gel rubber pearl of gel effect can be obtained.
Embodiment 10:
It is formulated according to embodiment 1, water bath time is changed to 7min, and condition is constant.This case is prepared according to the step of embodiment 1
The chitosan gel rubber pearl for the capsule shape that example is implemented.The dosage of sodium β-glycerophosphate pentahydrate is 1.4g, medium viscosity chitosan
Dosage is 0.4g, acetate concentration 0.1mol/L, adjusts pH value between 6.9-7.1, and lauryl sodium sulfate dosage is 0.2g,
Curing time is 1h, and bath temperature is 42 DEG C.Also the excellent chitosan gel rubber pearl of gel effect can be obtained.
Embodiment 11:
It is formulated according to embodiment 1, pH adjusting agent is changed to dipotassium hydrogen phosphate, condition is constant.The step of according to embodiment 1
Prepare the chitosan gel rubber pearl for the capsule shape that present case is implemented.The dosage of sodium β-glycerophosphate pentahydrate is 1.4g, medium viscosity
The dosage of chitosan is 0.4g, acetate concentration 0.1mol/L, adjusts pH value between 6.9-7.1, lauryl sodium sulfate is used
Amount is 0.2g, and curing time 1h, bath temperature is 42 DEG C, water bath time 5min.Also the excellent shell of gel effect can be obtained
Polysaccharide gel pearl.
Embodiment 12:
It is formulated according to embodiment 1, change sodium β-glycerophosphate quality is 1.6g, and condition is constant.According to the step of embodiment 1
The chitosan gel rubber pearl for the capsule shape that rapid preparation present case is implemented.The dosage of medium viscosity chitosan is 0.4g, and acetate concentration is
0.1mol/L adjusts pH value between 6.9-7.1, and lauryl sodium sulfate dosage is 0.2g, curing time 1h, bath temperature
It is 42 DEG C, water bath time 5min.Also the excellent chitosan gel rubber pearl of gel effect can be obtained.
Embodiment 13:
It is formulated according to embodiment 1, change sodium β-glycerophosphate quality is 1.4g, and condition is constant.According to the step of embodiment 1
The chitosan gel rubber pearl for the capsule shape that rapid preparation present case is implemented.The dosage of medium viscosity chitosan is 0.4g, and acetate concentration is
0.1mol/L adjusts pH value between 6.9-7.1, and lauryl sodium sulfate dosage is 0.2g, curing time 1h, bath temperature
It is 42 DEG C, water bath time 5min.Also the excellent chitosan gel rubber pearl of gel effect can be obtained.
Embodiment 14:
It is formulated according to embodiment 1, change sodium β-glycerophosphate quality is 1.2g, and condition is constant.According to the step of embodiment 1
The chitosan gel rubber pearl for the capsule shape that rapid preparation present case is implemented.The dosage of medium viscosity chitosan is 0.4g, and acetate concentration is
0.1mol/L adjusts pH value between 6.9-7.1, and lauryl sodium sulfate dosage is 0.2g, curing time 1h, bath temperature
It is 42 DEG C, water bath time 5min.Also the excellent chitosan gel rubber pearl of gel effect can be obtained.
Embodiment 15:
It is formulated according to embodiment 1, changing SDS receiving liquid mass fraction is 1%, and condition is constant.According to the step of embodiment 1
The chitosan gel rubber pearl for the capsule shape that rapid preparation present case is implemented.The dosage of sodium β-glycerophosphate pentahydrate be 1.4g, in glue
The dosage for spending chitosan is 0.4g, acetate concentration 0.1mol/L, adjusts pH value between 6.9-7.1, lauryl sodium sulfate
Dosage is 0.2g, and curing time 1h, bath temperature is 42 DEG C, water bath time 5min.Also it is excellent that gel effect can be obtained
Chitosan gel rubber pearl.
Embodiment 16:
It is formulated according to embodiment 1, changing SDS receiving liquid mass fraction is 2%, and condition is constant.According to the step of embodiment 1
The chitosan gel rubber pearl for the capsule shape that rapid preparation present case is implemented.The dosage of sodium β-glycerophosphate pentahydrate be 1.4g, in glue
The dosage for spending chitosan is 0.4g, acetate concentration 0.1mol/L, adjusts pH value between 6.9-7.1, lauryl sodium sulfate
Dosage is 0.8g, and curing time 1h, bath temperature is 42 DEG C, water bath time 5min.Also it is excellent that gel effect can be obtained
Chitosan gel rubber pearl.
Embodiment 17:
It is formulated according to embodiment 1, changing SDS receiving liquid mass fraction is 4%, and condition is constant.According to the step of embodiment 1
The chitosan gel rubber pearl for the capsule shape that rapid preparation present case is implemented.The dosage of sodium β-glycerophosphate pentahydrate be 1.4g, in glue
The dosage for spending chitosan is 0.4g, acetate concentration 0.1mol/L, adjusts pH value between 6.9-7.1, lauryl sodium sulfate
Dosage is 0.8g, and curing time 1h, bath temperature is 42 DEG C, water bath time 5min.Also it is excellent that gel effect can be obtained
Chitosan gel rubber pearl.
2. the preparation method that chitosan gel rubber pearl contains small molecule:
Embodiment 18:
The chitosan of pH value/(CS/ β-GP is molten for sodium β-glycerophosphate pentahydrate mixed solution is regulated in Example 1
Liquid), the Fluress that 1mL mass fraction is 1mg/L is added dropwise thereto.After stirring is completely dispersed it, remaining preparation step
It is rapid in the same manner as in Example 1.The chitosan gel rubber pearl for having coated fluorescein sodium is placed 12 hours in water, is revealed without obvious,
It contains and works well, as shown in Figure 2.
Embodiment 19:
The chitosan of pH value/(CS/ β-GP is molten for sodium β-glycerophosphate pentahydrate mixed solution is regulated in Example 1
Liquid), the rhodamine B solution that 1mL mass fraction is 1mg/L is added dropwise thereto.After stirring is completely dispersed it, remaining preparation step
It is in the same manner as in Example 1.It is revealed after placing 12h without obvious, contains and work well.
Claims (6)
1. a kind of preparation method of chitosan gel rubber pearl, it is characterised in that: first by the mixing of chitosan and sodium β-glycerophosphate
Solution is added drop-wise in anionic surfactant solution by liquid-transfering gun, solidifying based on chitosan and anionic surfactant
Poly- effect, forming core material, there are also the chitosan capsules of chitosan and sodium β-glycerophosphate；Then, by heating, make capsule
Chitosan and sodium β-glycerophosphate by hydrogen bond action, form gel, finally obtain chitosan gel rubber pearl；
Method includes the following steps:
(1) chitosan/sodium β-glycerophosphate pentahydrate mixed solution preparation:
1.2g-1.6g sodium β-glycerophosphate pentahydrate is dissolved in 2mL water, and the medium viscosity chitosan of 0.4g is dissolved in
In the acetum of 0.1mol/L；Under ice-water bath, sodium β-glycerophosphate five is slowly added dropwise into the chitosan solution dissolved
Hydrate soln obtains chitosan/sodium β-glycerophosphate pentahydrate mixed solution, is referred to as CS/ β-GP mixed solution；Institute
The medium viscosity chitosan stated, viscosity are 200-400mPa.s, deacetylation >=90%；
(2) chitosan/adjusting of sodium β-glycerophosphate pentahydrate mixed solution pH value and the system of sodium dodecyl sulfate solution
It is standby:
It weighs 25g disodium hydrogen phosphate solid to be dissolved in 100ml water, dissolves the disodium phosphate soln being saturated；To CS/ β-GP
The disodium phosphate soln of mixed solution and dripping saturation adjusts pH value between 6.9-7.1；Weigh 0.2g-0.8g dodecyl
Solid sodium sulfate is dissolved in 20mL water, is prepared the lauryl sodium sulfate receiving liquid of mass fraction 1%-4%, is referred to as SDS
Receiving liquid；
(3) preparation of chitosan gel rubber pearl:
It is instilled in SDS receiving liquid with liquid-transfering gun by the CS/ β-GP solution that pH value is 6.9-7.1 is regulated, it is poly- that shell is obtained after curing
Then sugared microcapsules are washed with distilled water 3 times, place into water-bath and heat, the CS/ β-GP solution inside microcapsules is changed into
Gel, to obtain chitosan gel rubber pearl.
2. the preparation method of chitosan gel rubber pearl according to claim 1, it is characterised in that: instill CS/ β-GP solution
In SDS receiving liquid, curing time 50-70min.
3. the preparation method of chitosan gel rubber pearl according to claim 1, it is characterised in that: chitosan microcapsules are changed into
When gel beads, bath temperature is 39-45 DEG C, water bath time 4-7min.
4. the preparation method of chitosan gel rubber pearl according to claim 1, it is characterised in that: chitosan and β-phosphoglycerol
The mass ratio of sodium is 1/3-1/4.
5. the application for the chitosan gel rubber pearl that in Claims 1-4 prepared by any claim the method, it is characterized in that the shell
Polysaccharide gel pearl is containing the application in small molecule dyes.
6. application according to claim 5, it is characterised in that: the chitosan gel rubber pearl is to molecular weight between 350-800
Small molecule dyes have excellent containing property, place 12 hours without obvious leakage, have and good contain stability.
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| CN107855080B (en) * | 2017-10-30 | 2020-09-08 | 中国科学院过程工程研究所 | Polymer gel particle, preparation method thereof, composite gel particle containing polymer gel particle and application |
| CN109627499B (en) * | 2018-11-30 | 2020-11-27 | 湖南工业大学 | Preparation method of biomass composite gel with shear thickening effect |
| CN109912251A (en) * | 2019-02-27 | 2019-06-21 | 南昌大学 | Fluorescent marker microcapsules and preparation method for cement matrix crack detection reparation |
| CN115089510B (en) * | 2022-06-20 | 2023-03-28 | 江南大学 | Intelligent temperature-sensitive permanent wave agent capable of reducing thioglycollic acid substances from entering human body and preparation method thereof |
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| CN103721655A (en) * | 2014-01-06 | 2014-04-16 | 武汉理工大学 | Preparation method of chitosan microcapsule with uniform size and controllable size |
| CN105147597A (en) * | 2015-10-28 | 2015-12-16 | 青岛高新区尚达医药研究所 | Thermo-sensitive marine organism gel |
| CN106040120A (en) * | 2016-05-24 | 2016-10-26 | 武汉理工大学 | Preparation method for SiO2 nanoparticle reinforced chitosan composite microcapsule |
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| CN103721655A (en) * | 2014-01-06 | 2014-04-16 | 武汉理工大学 | Preparation method of chitosan microcapsule with uniform size and controllable size |
| CN105147597A (en) * | 2015-10-28 | 2015-12-16 | 青岛高新区尚达医药研究所 | Thermo-sensitive marine organism gel |
| CN106040120A (en) * | 2016-05-24 | 2016-10-26 | 武汉理工大学 | Preparation method for SiO2 nanoparticle reinforced chitosan composite microcapsule |
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