CN109908846A - A kind of microcapsules and its preparation method and application - Google Patents
A kind of microcapsules and its preparation method and application Download PDFInfo
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Abstract
The present invention provides a kind of microcapsules and its preparation method and application, and the wall material of the microcapsules includes isocyanates and nano-titanium dioxide.Wall material of the isocyanates as microcapsules is selected, under emulsifier and mechanical shearing effect, core material is made to form submicron order oil droplet, curing agent is added, wall material occurs polymerization in oil droplets and coated, and nano-TiO is added during cyst wall formation2Dispersion liquid makes it load to cyst wall surface.The preparation method of microcapsules provided by the present invention can realize the microencapsulation of essential oil, it can promote the release of fragrance under solar radiation, experiment flow is obviously shortened compared with the prior art, synthesis process is without adjusting solution acid alkalinity, microcapsules can be dry by heat drying after being simply centrifuged, partial size integrated distribution is at 0.581 μm or so, and essential oil embedding rate is 78.8%, and three months essential oil retention rates of room temperature storage are up to 92.13%.
Description
Technical field
The present invention relates to flavors and fragrances processing technique fields more particularly to a kind of microcapsules and its preparation method and application.
Background technique
Essential oil is the parts such as the flower from fragrant plant, leaf, root, skin, stem, branch, fruit, seed, takes distillation, squeezing, extraction
With the oily mater of characteristic perfume made from the methods of taking, adsorb.They are the mixtures of many compounds, mainly there is terpenes
Hydro carbons, arene, alcohols, aldehydes, ketone, ethers, esters and phenols etc..It, can when essential oil is used for the Aroma finishing of textile
Assign clothing, pillow cover, the fabrics such as necktie to calm the nerves, calmness, hypnosis, the even health-care efficacies such as physical therapy, special aromatic odor
People can also be made to be in a cheerful frame of mind, cover bad smell, improve self-image.But it the disadvantages of volatile, unstable due to its, leads
Cause fragrance remaining time short, to limit the development and utilization and development of essential oil.
Embedding treatment is carried out to essential oil using microencapsulation technology, is research hotspot in recent years.Microencapsulation technology is
Core material is improved to light, heat, the stability of oxygen using the embedding effect of wall material, controls the moisture absorption of core material, reduces the volatilization damage of core material
It loses, to assign the function of the lasting lasting of essential oil.But the preparation process of existing microcapsules is more complex at present, synthesis condition
It is required that it is harsh, it cannot achieve industrialized production, and the Microcapsules Size size prepared is larger, particle diameter distribution is uneven, microcapsules
Structure is imperfect, poor so as to cause the stability of microcapsules, and lasting lasting function is not good enough.
Summary of the invention
It is complicated for existing essential oil microcapsules preparation process, the capsule size being prepared it is larger and be unevenly distributed with
And the imperfect problem for causing microcapsule stability poor of microcapsule structure, the present invention provide a kind of essential oil microcapsules and its preparation
Methods and applications.
In order to solve the above technical problems, present invention provide the technical scheme that
A kind of microcapsules, including core material and wall material, the wall material include isocyanates and nano-titanium dioxide.
Traditional microcapsules need just cyst wall be made to rupture, to discharge capsule-core by mechanical or heating etc. mode
In substance, the present invention in nano-titanium dioxide under illumination condition, can promote-the C-N in cyst wall polyurethane formic acid ester structure
=O fracture generates NH4 +, NH4 +And then it is oxidized to NO3 -, cause cyst wall to rupture, be conducive to the release of capsule-core substance, to reach
Regulate and control the purpose of release.And the load nano-titanium dioxide on cyst wall, the mechanical property of cyst wall can be increased, improve the steady of microcapsules
It is qualitative, core material is protected, preferably so as to improve the sustained release performance of microcapsules.
Isocyanates of the present invention includes but are not limited to isopropyl isocyanate, two isocyanide of tri-methyl hexamethylene
Acid esters, 1,4- cyclohexane diisocyanate, tetramethylene diisocyanate, 2,6- toluene di-isocyanate(TDI), hexa-methylene two are different
The biuret of cyanate, the tripolymer of isophorone diisocyanate, the tripolymer of hexamethylene diisocyanate, 4,4 ', 4 "-
The common isocyanates such as triphenylmethane triisocyanate.
Preferably, the isocyanates is hexamethylene diisocyanate trimer.
Compared with prior art, the present invention selects wall material of the hexamethylene diisocyanate trimer as microcapsules,
Degree of polymerization height and heat-resist polyurethane are formed after solidification, make cyst wall that there is better compactness and integrality, so as to more
Good protection core material, prevents core material from leaking.
Preferably, the core material is oily compound.
It is furthermore preferred that the core material is essential oil or compound essence.
The present invention does not have special limitation to the type of the essential oil and compound essence and source, using those skilled in the art
Aromatics plants essential oil or essence known to member.
Preferably, the mass ratio of the isocyanates and nano-titanium dioxide is 400-600:1.
Preferably, the mass ratio of the isocyanates and the core material is 1:0.8-1.2.
The mass ratio of the mass ratio and wall material and nano-titanium dioxide of preferred wall material and core material, can be such that microcapsules have
There are preferable integrality and sustained release performance, controllable release performance.
Preferably, the partial size of the nano-titanium dioxide is 25-35nm.
The partial size of preferred nano-titanium dioxide, can make titanium dioxide have preferable photocatalysis effect, promote cyst wall
Rupture, thus under illumination condition capsule-core substance release.
The present invention also provides a kind of preparation methods of microcapsules, include the following steps:
Step 1: the design proportion according to above-mentioned microcapsules weighs the isocyanates and core material, emulsifier water is added
Solution is emulsified under conditions of stirring shearing, obtains emulsion；
Step 2: curing agent is added dropwise in Xiang Suoshu emulsion, continues after being added dropwise under conditions of 70-80 DEG C of stirring
50-70min is stirred, nano titanium oxide dispersion is added dropwise, continues to stir 50-70min, be centrifuged, drying obtains microcapsules.
Preparing wall material selected by the common process of microcapsules is generally solid, need to be performed under heating conditions dissolution or melt
Change, it is longer the time required to process；Harshness is required to the pH value of reaction solution in microcapsules synthesis process, pH is too high or too low,
It needs to carry out residual titration, to cause very big influence to microcapsules molding.
It is wall material that the present invention, which selects liquid hexamethylene diisocyanate trimer, without being dissolved by heating, is solidified
The polyurethane formed afterwards is right high and heat-resist, and the microcapsules being prepared only are needed by simple centrifugation and ordinary hot
Wind product obtained by drying, needs not move through traditional vacuum freeze drying；And without adjusting pH value in preparation process, in original solution
In the curing moldings of sub-micron partial size microcapsules can be realized, avoid impacting microcapsules molding because pH is too high or too low.
Compared with the conventional method, the preparation method of microcapsules provided by the invention only need to be emulsified simply, solidified, is centrifuged, be dried
Microcapsules solid powder can be obtained, has process short, easy to operate, the advantages such as at low cost.
Preferably, in step 1, the stirring is cut into is sheared while agitating, shear velocity 4500-
5000r/min shears 8-12min, rises to 10000-12000r/min, shears 7-10min；Shear history mixing speed is 550-
600r/min。
Optionally, stirring is stirred using magnetic force, and shearing is using conventional emulsification cutting head.
Specifically, adding after emulsifier aqueous solution is added in hexamethylene diisocyanate trimer and oily compound
Enter magnetic force, cutting head is submerged in solution, is raised speed with the speed of 500r/min per second to 4500-5000r/min, shearing terminates
Afterwards with the speed reduction of speed of 500r/min per second, speed-raising time and deceleration time are not counted in shear time.
Due to the stirring of bottom magnetic force and the shearing collective effect on top, solution in container is made to be in constantly circulation fortune
Dynamic, the effect of the biggish oily compound drop meeting stress of top volume is towed to shearing position, forms the liquid of small volume
Since magnetic agitation keeps its evenly dispersed in the solution after drop, the uniform emulsion of submicron order droplet size is formed.
Preferred emulsion process, substantially reduces the time of convention stir emulsification grease mixed phase, while also improving institute
It is big to avoid convention stir emulsification bring particle size distribution partial size wide, not easy to control for the homogeneity for forming drop size
The problems such as small, so that Microcapsules Size narrowly distributing has been prepared, particle size is simply controllable.Micro- glue that the present invention is prepared
The partial size of capsule below can reach 80% or more at 1 μm.
Preferably, in step 1, the concentration of the emulsifier aqueous solution is 0.01-0.02g/ml.
Emulsifier aqueous solution refers to the aqueous solution of emulsifier in the present invention.
Preferably, the mass ratio of the emulsifier aqueous solution and the core material is 13-15:1.
The concentration and dosage of preferred emulsifier aqueous solution, can make the oily compound in capsule-core fully emulsified, be formed steady
Fixed oil-in-water emulsion.
Preferably, the mass ratio of the curing agent and the isocyanates is 1:1-3.
The ratio of preferred curing agent and isocyanates, is conducive to the abundant solidification of wall material isocyanates, and it is complete to form structure
Whole microcapsules.
Preferably, the content of titanium dioxide is 0.4-0.6wt% in the nano titanium oxide dispersion.
The concentration of preferred nano-titanium dioxide is conducive to improve the dispersion degree of titanium dioxide granule, to be conducive to dioxy
Change on titanium nano particle uniform load cyst wall.
Preferably, in step 2, mixing speed 650-700r/min.
Preferably, in step 2, the rate of addition of curing agent is 15-20 μ L/s.
The rate of addition of preferred curing agent can reduce the blocky aggregation of microcapsules, cooperate low temperature drying, after can making drying
Microcapsules without grinding only by rubbing can shape solid powder, and separating degree is high, and no adhesion phenomenon simplifies microcapsules
Preparation process.
Preferably, in step 2, the rate of addition of nano titanium oxide dispersion is 15-20 μ L/s.
The rate of addition of preferred nano-titanium dioxide can make titania nanoparticles uniform load in the capsule of microcapsules
On wall.
Preferably, in step 2, drying temperature is 75-85 DEG C, drying time 30-40min.
The above-mentioned microcapsules being prepared 75-85 DEG C of drying 30-40min in a conventional oven takes out, is down to room naturally
Temperature.Preferred drying mode can slow down the rapid evaporation of solution, avoid blocky adhesion after traditional high polymer microcapsules are dried
Phenomenon is serious, need to carry out the appearance of grinding separation problem；Meanwhile drying temperature is lower, avoid traditional spray drying due to
Vapo(u)rizing temperature height (generally higher than 180 DEG C), and the appearance of the volatilization of capsule-core substance and loss problem is caused, it is the micro- of thermal sensitivity core material
The preparation of capsule product provides a kind of new technological means guidance.
Preferably, it is 85-90% that emulsifier, which is alcoholysis degree, and the degree of polymerization is the polyvinyl alcohol of 1600-1800.
Preferred emulsifier has the advantages that preferable acid and alkali-resistance, grease and lubricant corrode, oily compound can be made to fill
Divide emulsification, form stable oil-in-water emulsion, keeps the microcapsule embedded rate obtained high, product surface is uniform, reaches superior
Embed effect.
Preferably, the curing agent is 1,3-BDO.
Preferred curing agent can be such that isocyanates sufficiently polymerize, and form the microcapsules of structural integrity.
The partial size integrated distribution of the microcapsules obtained by above-mentioned preparation method at 0.581 μm or so, oily compound
Embedding rate can reach 78.8% or more, and the retention rate of oily compound is up to 92% or more in three months capsule-cores of room temperature storage.On
The simple process of preparation essential oil microcapsules is stated, the size of mild condition, the microcapsules being prepared is smaller, and separating degree is high, stablizes
Property it is good, it is low in cost, be suitable for enterprise be mass produced.
The present invention also provides application of the above-mentioned microcapsules in textile Aroma finishing agent.
Microcapsules in the present invention are applied to the agent of textile Aroma finishing, in fabric softener, clothing can be made fragrant
Persistently, especially summer, perspiring is more, is easy to appear peculiar smell, and micro- glue can be improved in microcapsules provided by the invention in the sunlight
The ability of capsule fragrance release improves self-image to cover bad smell well.
Detailed description of the invention
Fig. 1 is the photo of microcapsule product prepared by the embodiment of the present invention 1；
Fig. 2 is the photo of the microcapsule product of comparative example 1 of the present invention preparation；
Fig. 3 is the scanning electron microscopic picture of microcapsule product prepared by the embodiment of the present invention 1；
Fig. 4 is the scanning electron microscopic picture of the microcapsule product of comparative example 1 of the present invention preparation；
Fig. 5 is the grain size distribution of microcapsule product prepared by the embodiment of the present invention 1；
Fig. 6 is the grain size distribution of the microcapsule product of comparative example 1 of the present invention preparation；
Fig. 7 is the transmission electron microscope picture of microcapsule product prepared by the embodiment of the present invention 1；
Fig. 8 micro- glue in the case where having illumination and non-illuminated conditions for the embodiment of the present invention 1 and the microcapsule product of the preparation of comparative example 1
The comparison diagram of capsule fragrance releasing effect.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Embodiment 1
A kind of preparation method of microcapsules:
It is added in 100ml beaker Step 1: weighing polyvinylalcohol solids 1g, 70ml distilled water is added, places the beaker 30
In DEG C water-bath, with the speed magnetic agitation 5min of 600r/min, emulsifier aqueous solution is obtained；
Step 2: weighing hexamethylene diisocyanate trimer 5g and plain blue essential oil 5g, the emulsifier is added
Magnetic force is added in aqueous solution, in beaker, mixing speed 580r/min submerges cutting head in solution, with 500r/ per second
The speed of min slowly raises speed to 4800r/min, shears 10 minutes, rises to 11000r/min shearing 8min, obtains emulsion；
Step 3: the emulsion is placed in heat collecting type constant-temperature heating magnetic stirring apparatus, when emulsion temperature rises to 75 DEG C
When, under conditions of 680r/min, 1,3-BDO 2ml is added dropwise, rate of addition is 18 μ L/s, continues to stir after being added dropwise
The TiO of 0.5wt% is added dropwise in 1h2Dispersion liquid 2ml, rate of addition are 18 μ L/s, continue to stir 1h, obtain microcapsule solution；
Step 4: microcapsule solution is placed in centrifuge tube, 5min is centrifuged with the speed of 8000r/min, pours out supernatant,
Distilled water to pipe 2/3 is added to go out, ultrasound makes solid be uniformly dispersed, and continues to be centrifuged 5min, removes supernatant after secondary centrifuging, will
Microcapsules precipitating is put into 80 DEG C of drying 35min in electric heating constant-temperature blowing drying box together with centrifuge tube, then takes out, is down to naturally
Room temperature is to get microcapsules.
Embodiment 2
A kind of preparation method of microcapsules:
It is added in 100ml beaker Step 1: weighing polyvinylalcohol solids 1.5g, 70ml distilled water is added, places the beaker
In 30 DEG C of water-baths, with the speed magnetic agitation 5min of 600r/min, emulsifier aqueous solution is obtained；
Step 2: weighing hexamethylene diisocyanate trimer 4.6g and Rosa Damascana 5.5g, the emulsifier is added
Magnetic force is added in aqueous solution, in beaker, mixing speed 550r/min submerges cutting head in solution, with 500r/ per second
The speed of min slowly raises speed to 5000r/min, shears 8 minutes, rises to 12000r/min shearing 7min, obtains emulsion；
Step 3: the emulsion is placed in heat collecting type constant-temperature heating magnetic stirring apparatus, when emulsion temperature rises to 70 DEG C
When, under conditions of 650r/min, 1,3-BDO 4.6ml is added dropwise, rate of addition is 20 μ L/s, continues to stir after being added dropwise
The TiO of 0.5wt% is added dropwise in 50min2Dispersion liquid 2.3ml, rate of addition are 20 μ L/s, continue to stir 70min, it is molten to obtain microcapsules
Liquid；
Step 4: microcapsule solution is placed in centrifuge tube, 5min is centrifuged with the speed of 8000r/min, pours out supernatant,
Distilled water to pipe 2/3 is added to go out, ultrasound makes solid be uniformly dispersed, and continues to be centrifuged 5min, removes supernatant after secondary centrifuging, will
Microcapsules precipitating is put into 85 DEG C of drying 30min in electric heating constant-temperature blowing drying box together with centrifuge tube, then takes out, is down to naturally
Room temperature is to get microcapsules.
Embodiment 3
A kind of preparation method of microcapsules:
It is added in 100ml beaker Step 1: weighing polyvinylalcohol solids 1.3g, 70ml distilled water is added, places the beaker
In 30 DEG C of water-baths, with the speed magnetic agitation 5min of 600r/min, emulsifier aqueous solution is obtained；
Step 2: weighing hexamethylene diisocyanate trimer 6g and Lavender 4.8g, the emulsifier is added
Magnetic force is added in aqueous solution, in beaker, mixing speed 600r/min submerges cutting head in solution, with 500r/ per second
The speed of min slowly raises speed to 4500r/min, shears 12 minutes, rises to 10000r/min shearing 10min, obtains emulsion；
Step 3: the emulsion is placed in heat collecting type constant-temperature heating magnetic stirring apparatus, when emulsion temperature rises to 80 DEG C
When, under conditions of 700r/min, 1,3-BDO 2ml is added dropwise, rate of addition is 15 μ L/s, continues to stir after being added dropwise
The TiO of 0.5wt% is added dropwise in 70min2Dispersion liquid 2ml, rate of addition are 15 μ L/s, continue to stir 50min, obtain microcapsule solution；
Step 4: microcapsule solution is placed in centrifuge tube, 5min is centrifuged with the speed of 8000r/min, pours out supernatant,
Distilled water to pipe 2/3 is added to go out, ultrasound makes solid be uniformly dispersed, and continues to be centrifuged 5min, removes supernatant after secondary centrifuging, will
Microcapsules precipitating is put into 75 DEG C of drying 40min in electric heating constant-temperature blowing drying box together with centrifuge tube, then takes out, is down to naturally
Room temperature is to get microcapsules.
The hexamethylene diisocyanate trimer that Jining Hua Kai resin Co., Ltd is selected in embodiment 1-3 is wall material,
Polyvinyl alcohol 1788 by selecting sub- safe joint Chemical Co., Ltd. is essential oil emulsifier, and selecting Shanghai to irrigate triumphant chemical reagent has
The 1,3-BDO of limit company is curing agent, selects 0.5% nano-titanium dioxide point of Beijing Fu Site new material Co., Ltd
Dispersion liquid.
Comparative example 1
A kind of preparation method of microcapsules:
It is added in 100ml beaker Step 1: weighing polyvinylalcohol solids 1g, 70ml distilled water is added, places the beaker 30
In DEG C water-bath, with the speed magnetic agitation 5min of 600r/min, emulsifier aqueous solution is obtained；
Step 2: weighing hexamethylene diisocyanate trimer 5g and plain blue essential oil 5g, the emulsifier is added
Magnetic force is added in aqueous solution, in beaker, mixing speed 580r/min submerges cutting head in solution, with 500r/ per second
The speed of min slowly raises speed to 4800r/min, shears 10 minutes, rises to 11000r/min shearing 8min, obtains emulsion；
Step 3: the emulsion is placed in heat collecting type constant-temperature heating magnetic stirring apparatus, when emulsion temperature rises to 75 DEG C
When, under conditions of 680r/min, 1,3-BDO 2ml is added dropwise, rate of addition is 18 μ L/s, continues to stir after being added dropwise
2h obtains microcapsule solution；
Step 4: microcapsule solution is placed in centrifuge tube, 5min is centrifuged with the speed of 8000r/min, pours out supernatant,
Distilled water to pipe 2/3 is added to go out, ultrasound makes solid be uniformly dispersed, and continues to be centrifuged 5min, removes supernatant after secondary centrifuging, will
Microcapsules precipitating is put into 80 DEG C of drying 35min in electric heating constant-temperature blowing drying box together with centrifuge tube, then takes out, is down to naturally
Room temperature is to get microcapsules.
Embodiment 1 prepare microcapsule product photo as shown in Figure 1, comparative example 1 prepare microcapsule product photo
As shown in Fig. 2, there is no blocky viscous it can be seen from the figure that high using the microcapsules separating degree that the method for the present invention is prepared
Even phenomenon.
The scanning electron microscopic picture of microcapsule product prepared by embodiment 1 is as shown in figure 3, microcapsules prepared by comparative example 1 produce
The scanning electron microscopic picture of product as shown in figure 4, it can be seen from the figure that by using microcapsules provided by the invention preparation method
It can get the microcapsules of the good submicron order polyurethane package essential oil of form, and microcapsules separating degree is high, encystation effect is good.
The grain size distribution of microcapsule product prepared by embodiment 1 is as shown in figure 5, microcapsule product prepared by comparative example 1
Grain size distribution as shown in fig. 6, it can be seen from the figure that the Microcapsules Size size integrated distribution that comparative example 1 is prepared
It is distributed in partial size in 0.739 μm or so, the capsule grain diameter set of dimensions that embodiment 1 is prepared and concentrates in partial size integrated distribution and divides
It is uniformly sub- to illustrate that the preparation method of the microcapsules provided through the invention can obtain particle diameter distribution at 0.581 μm or so for cloth
Micron essential oil microcapsules, and load TiO2Later microcapsules it is smaller, particle diameter distribution is more concentrated.
Embodiment 1 prepare microcapsule product transmission electron microscope picture as shown in fig. 7, it can be seen from the figure that
Titanium dioxide nanoparticle is equably supported on the cyst wall of microcapsules.
The test of essential oil retention rate
Example 1 and comparative example 1 prepare each 1g of products obtained therefrom in culture dish respectively, and it is transparent and not to put it into self-control
In transparent fragrance test box (length × width × height: 27cm × 22cm × 28cm), transparent fragrance test box is placed in illumination item
Under part, opaque fragrance test box is disposed within, essential oil retention rate situation of change under illumination simulation and non-illuminated conditions, uses
The fragrance value of XP-329m fragrance tester measurement different time, wherein embodiment 1 and comparative example 1 respectively do three groups of parallel tests.
Microcapsules fragrance discharges data under 1 illumination condition of table
Microcapsules fragrance discharges data under 2 non-illuminated conditions of table
Microcapsule product prepared by the embodiment of the present invention 1 and comparative example 1 microcapsules in the case where having illumination and non-illuminated conditions are fragrant
The comparison diagram of taste releasing effect is as shown in Figure 8.It can be seen from upper table and Fig. 8 under no light condition, embodiment 1 and comparative example 1
The microcapsules fragrance numerical value of preparation is closer to, it was demonstrated that microcapsules prepared by the present invention can completely wrap up essential oil, suppression
It makes it quickly to volatilize, solves the storage problem of essential oil.Under illumination condition, the fragrance value of microcapsules prepared by comparative example 1
Without significant change, fragrance value is significantly increased in microcapsules 2h prepared by embodiment 1, is then gradually decreased, but is still higher than common micro-
The release value of capsule, it is possible thereby to judge, the load TiO that illumination can promote embodiment 1 to prepare2Fragrance releases in microcapsules
It puts.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modification, equivalent replacement or improvement etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of microcapsules, including core material and wall material, which is characterized in that the wall material includes isocyanates and nanometer titanium dioxide
Titanium.
2. microcapsules as described in claim 1, which is characterized in that the isocyanates is hexamethylene diisocyanate trimerization
Body；And/or
The core material is oily compound.
3. microcapsules as described in claim 1, which is characterized in that the core material is essential oil or compound essence.
4. microcapsules as described in claim 1, which is characterized in that the mass ratio of the isocyanates and nano-titanium dioxide is
400-600:1；And/or
The mass ratio of the isocyanates and the core material is 1:0.8-1.2；And/or
The partial size of the nano-titanium dioxide is 25-35nm.
5. a kind of preparation method of microcapsules, which comprises the steps of:
Step 1: the design proportion according to the described in any item microcapsules of claim 1-4 weighs the isocyanates and core material,
Emulsifier aqueous solution is added, is emulsified under conditions of stirring shearing, obtains emulsion；
Step 2: curing agent is added dropwise in Xiang Suoshu emulsion, continues to stir after being added dropwise under conditions of 70-80 DEG C of stirring
Nano titanium oxide dispersion is added dropwise in 50-70min, continues to stir 50-70min, be centrifuged, and drying obtains microcapsules.
6. the preparation method of microcapsules as claimed in claim 5, which is characterized in that in step 1, the stirring is cut into
It is sheared while stirring, shear velocity 4500-5000r/min, shears 8-12min, rise to 10000-12000r/min,
Shear 7-10min；Mixing speed is 550-600r/min；And/or
The concentration of the emulsifier aqueous solution is 0.01-0.02g/ml.
7. the preparation method of microcapsules as claimed in claim 6, which is characterized in that the emulsifier aqueous solution and the core material
Mass ratio be 13-15:1；And/or
The mass ratio of the curing agent and the isocyanates is 1:1-3；And/or
The content of titanium dioxide is 0.4-0.6wt% in the nano titanium oxide dispersion.
8. the preparation method of microcapsules as claimed in claim 7, which is characterized in that in step 2, mixing speed 650-
700r/min；And/or
The rate of addition of curing agent is 15-20 μ L/s；And/or
The rate of addition of nano titanium oxide dispersion is 15-20 μ L/s；And/or
Drying temperature is 75-85 DEG C, drying time 30-40min.
9. the preparation method of microcapsules as claimed in claim 7, which is characterized in that emulsifier is that alcoholysis degree is 85-90%, is gathered
The right polyvinyl alcohol for 1600-1800；And/or
The curing agent is 1,3 butylene glycol.
10. application of the described in any item microcapsules of claim 1-4 in textile Aroma finishing agent.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112691622A (en) * | 2020-12-07 | 2021-04-23 | 绍兴文理学院元培学院 | Nitrogen-doped nano titanium dioxide/aromatic microcapsule and preparation method and application thereof |
| CN115746954A (en) * | 2022-10-24 | 2023-03-07 | 湖北中烟工业有限责任公司 | Emulsified essence, preparation method thereof and perfuming tube |
| CN116920737A (en) * | 2023-07-20 | 2023-10-24 | 武汉纺织大学 | Silicon dioxide-polyurethane composite phase-change microcapsule and preparation method thereof |
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| ANTÓNIO D. RIBEIRO ET AL.: ""Microencapsulation of citronella oil for solar-activated controlled release as aninsect repellent"", 《APPLIED MATERIALS TODAY》 * |
| NUSAIBA K. AL-NEMRAWI* ET AL.: ""Synthesis and Characterization of Photocatalytic Polyurethane and Poly(Methyl Methacrylate) Microcapsules for the Controlled Release of Methotrexate"", 《DRUG DEVELOPMENT AND INDUSTRIAL PHARMACY》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112691622A (en) * | 2020-12-07 | 2021-04-23 | 绍兴文理学院元培学院 | Nitrogen-doped nano titanium dioxide/aromatic microcapsule and preparation method and application thereof |
| CN112691622B (en) * | 2020-12-07 | 2022-06-17 | 绍兴文理学院元培学院 | Nitrogen-doped nano titanium dioxide/aromatic microcapsule and preparation method and application thereof |
| CN115746954A (en) * | 2022-10-24 | 2023-03-07 | 湖北中烟工业有限责任公司 | Emulsified essence, preparation method thereof and perfuming tube |
| CN116920737A (en) * | 2023-07-20 | 2023-10-24 | 武汉纺织大学 | Silicon dioxide-polyurethane composite phase-change microcapsule and preparation method thereof |
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| CN109908846B (en) | 2021-06-08 |
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