CN104593151A - Essence nanocapsule taking polyurea as capsule wall and preparation method of essence nanocapsule - Google Patents
Essence nanocapsule taking polyurea as capsule wall and preparation method of essence nanocapsule Download PDFInfo
- Publication number
- CN104593151A CN104593151A CN201510030379.5A CN201510030379A CN104593151A CN 104593151 A CN104593151 A CN 104593151A CN 201510030379 A CN201510030379 A CN 201510030379A CN 104593151 A CN104593151 A CN 104593151A
- Authority
- CN
- China
- Prior art keywords
- essence
- polyureas
- nano capsule
- nanocapsule
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
- B01J13/16—Interfacial polymerisation
Abstract
The invention provides an essence nanocapsule taking polyurea as a capsule wall and a preparation method of the essence nanocapsule. The essence nanocapsule taking polyurea as the capsule wall is characterized by being prepared from an oil-phase component and a water-phase component, wherein the oil-phase component comprises the following components: 5.0-20.0wt% of essence and 2.5-4.5wt% of diisocyanate; the water-phase component comprises the following components: 0.5-5.0wt% of an emulsifier, 0.5-2.5wt% of diamine and 68.0-91.5wt% of deionized water; and the weight percent sum of all the components is 100%. According to the essence nanocapsule, coating and controllable preparation of mint essence with the nanocapsule are realized for the first time; polyuria is used as the capsule wall to be encapsulated to prepare the nanocapsule; the heat stability and the slow-release effect of the capsule can be improved; meanwhile, the dispersity, the compatibility, the stability and the durability can be further improved; the product appearance of the nanocapsule can be kept invariable due to the transparency of nanometer effect; and the essence nanocapsule can be applied to the field of daily chemicals such as detergents, liquid shampoo and bath foam.
Description
Technical field
The invention belongs to capsule of nano field, particularly a kind of take polyureas as essence Nano capsule of cyst wall and preparation method thereof.
Background technology
Namely essence Nano capsule is the nano-grade capsule of capsule-core with essence.Essence is grouped into primarily of the one-tenth that alcohol, acid anhydride, ester, ketone etc. tens kinds are different, and their physical properties is same hardly, so more difficult in the process preparing microcapsule.Essence microcapsuleization can overcome the impact of many extraneous factors on essence, comprises the change of pH value, the change of pressure, the change etc. of temperature.By encapsulated, cyst wall plays a protective role to essence, and volatilization loss is suppressed, and fragrance retains complete, thus the stability that improve essence storage and use, and the effect of Co ntrolled release can be reached, product fragrance can be made lasting.Encapsulatedly can also improve the oxytolerant of essence, heat-resisting, fast light ability, strengthen the stability of capsule-core material.On the other hand essence is made capsule, the physical condition of essence can be changed thus to make it use in the industrial production more convenient.
Essence, as a kind of synthetic flavour, is the concentrated perfume oil of imitation fruit by synthetic and natural perfume smell, is applied to the industries such as food, daily use chemicals, tobacco, medicine more, closely bound up with daily life.Wherein peppermint essence is as application one of essence more widely, has very wide Application Areas: be applied to medicine, can make aromatic drug, remedium corrigens and carminative, for skin or mucous membrane, can produce refrigerant sense and be not suitable for alleviate, main pain; Be applied to field of food and can be used as additive, such as dessert, candy, milk etc.; Be applied to daily chemical products, spearmint oil can also be used for removing peculiar smell, clean ability to speak, such as toothpaste, chewing gum, bathing agents, cigarette etc.Take polyureas as the coated volatile Peppermint Oil of wall material, its thermostability can be made to be greatly improved, reach slow release effect at relatively high temperatures, the physicochemical property that its higher wear resistance etc. are excellent also contributes to the raising of essence slow release effect.
Summary of the invention
It take polyureas as essence Nano capsule of cyst wall and preparation method thereof that technical problem to be solved by this invention is to provide a kind of, peppermint essence is that a kind of volatility is very strong and the essence and flavoring agent that wetting ability is higher, and the essence Nano capsule in the present invention achieves the encapsulated of peppermint essence and makes Nano capsule, its thermostability and slow release effect can be improved, its dispersiveness, consistency, stability and persistence can be improved further simultaneously.Preparation technology of the present invention is simple and convenient, and the Nano capsule of preparation also can make product appearance remain unchanged due to the transparency that nano effect possesses, and household chemicals fields such as washing composition, shampoo, bathing agents that are applied to it have important practical value.
In order to solve the problems of the technologies described above, the invention provides a kind of take polyureas as the essence Nano capsule of cyst wall, it is characterized in that, is made up of oil phase component and water phase components; Described oil phase component is made up of essence 5.0 ~ 20.0wt% and vulcabond 2.5 ~ 4.5wt%; Described water phase components is made up of emulsifying agent 0.5 ~ 5.0wt%, diamines 0.5 ~ 2.5wt% and deionized water 68.0 ~ 91.5wt%, and the weight percent sum of all components is 100%.
Preferably, described essence is Peppermint Oil.Peppermint Oil is a kind of water-fast liquid essence.
Preferably, described vulcabond is 4, one or both in 4 '-diphenylmethanediisocyanate MDI and isophorone diisocyanate IPDI.
Preferably, described emulsifying agent is D-425.
Preferably, described diamines is 1,6-hexane diamines (HMDA).
Present invention also offers above-mentioned take polyureas as the preparation method of the essence Nano capsule of cyst wall, it is characterized in that, comprising:
Step 1: take each oil phase component and water phase components by weight percentage, preparation mass percent concentration is the emulsifier aqueous solution of 2-20%; Compound concentration is 8 ~ 40wt% bis-amine aqueous solution; By emulsifier aqueous solution and the mixing of remaining deionized water, obtain aqueous phase;
Step 2: by vulcabond and essence mixing, be stirred to and dissolve each other completely, obtained oil phase;
Step 3: under normal temperature, the oil phase of step 2 gained is joined in the aqueous phase of step 1 gained, clarifixator or homogenizer is used to carry out emulsification 3 ~ 5min, obtain primary emulsifying o/w emulsion, this emulsion is placed in ultrasonic cell disruptor and carries out ultrasonication, obtain the o/w emulsion after ultrasonic wave dispersion;
Step 4: the o/w emulsion after above-mentioned ultrasonic wave dispersion is placed in constant temperature blender with magnetic force, two amine aqueous solutions of preparation in step 1 are dripped under 30 ~ 40 DEG C of water-baths, heat up after constant temperature 20 ~ 30min, constant temperature 1.5 ~ 2.5h at 50 ~ 60 DEG C, is namely able to the essence Nano capsule that polyureas is cyst wall.
Preferably, when the use clarifixator in described step 3 carries out emulsification, shearing rate is 4000 ~ 9000rpm.
Preferably, the ultrasonic time in described step 3 is 20min ~ 40min, and ultrasonic power is 30% ~ 60% (total power is 900W).
The present invention utilizes interfacial polymerization to prepare with polyureas to be the essence Nano capsule of cyst wall.The polyurea shell of essence Nano capsule is formed by vulcabond and diamines polymerization reaction take place, and peppermint essence is then wrapped by as core.In preparation, aqueous phase is the water soluble emulsifier aqueous solution, diamines and deionized water, and oil phase is vulcabond, Peppermint Oil.After the mixing of aqueous phase, oil phase, high speed shear forms O/w emulsion, emulsion is placed in ultrasonic cell disruptor and carries out ultrasonication amount of time, obtain uniform and stable miniemulsion, vulcabond and diamines polymerization reaction take place on water oil interface forms polyurea shell, is coated on wherein by peppermint essence.
The interfacial polymerization principle applied is as follows:
Interfacial polymerization is dissolved in inconsistent two-phase respectively by two or more incompatible wall material monomer, core disperses or emulsification in the external phase being dissolved with reaction monomers, and on the surface of capsule-core, two kinds of wall material monomer polymerization reaction take places generate polymer shell wall and form microcapsule.One of important method that interfacial polymerization is prepared as microcapsule and Nano capsule, has the advantages such as speed of response is fast, mild condition, preparation method are simple and convenient.
The process that vulcabond and diamine reactant generate polyureas is polyaddition, specific as follows:
Isocyanato in vulcabond and the amino generation addition reaction in diamines generate urea groups, and polymolecular vulcabond is polymerized with diamines and forms polyureas, and reaction equation is as follows:
Compared with prior art, the invention has the beneficial effects as follows:
1, the present invention to be polymerized with diamines with vulcabond to form polyureas for shell, and with peppermint volatile oil for core, preparing a kind of take polyureas as the essence Nano capsule of cyst wall.Volatility is very strong and have and obtain effectively coated compared with the peppermint essence and flavoring agent of high-hydrophilic because of the polyureas cyst wall that polyreaction generates.Encapsulated by polyureas, play a protective role to essence, volatilization loss is suppressed, the stability that improve essence storage and use, and can reach the effect of Co ntrolled release, and product fragrance can be made lasting.On the other hand essence is made capsule, the physical condition of essence can be changed thus to make it use in the industrial production more convenient.
2, compared with microcapsule, make the polyureas Nano capsule being of a size of nanometer range, can further improve its thermostability, wear resistance and slow release effect, its consistency, stability and persistence can be improved further simultaneously.Nano capsule also can make product appearance remain unchanged due to the transparency that nano effect possesses.Mint Essence Nano capsule prepared by the present invention has good dispersiveness in water, and the fields such as household chemicals field and food, makeup, additive such as washing composition, shampoo, bathing agents that are applied to it have important practical value.
3, peppermint essence is that a kind of volatility is very strong and the essence and flavoring agent that wetting ability is higher, and the present invention achieves Nano capsule first to the coated of peppermint essence and controlled synthesis thereof.Polyureas carries out encapsulated as cyst wall and makes Nano capsule, thermostability and the slow release effect of capsule can be improved, its dispersiveness, consistency, stability and persistence can be improved further simultaneously, Nano capsule also can make product appearance remain unchanged due to the transparency that nano effect possesses, and can be applied to the household chemicals fields such as washing composition, shampoo, bathing agents.
4, preparation method of the present invention has high covering amount, and technique is simple and convenient, is easy to control, and the Nano capsule size prepared is little, even particle size distribution, has the advantages such as Heat stability is good, abrasive wear resistance are high, had good sustained release effect.The Nano capsule of preparation is capsule-core with Mint Essence, has the pharmaceutical use of blending value and certain peppermint.The present invention, while improve the value benefit of capsule, too increases its value added in household chemicals, meets the pursuit trend of people to material demand.
Accompanying drawing explanation
Fig. 1 is the essence Nano capsule of the embodiment of the present invention 1,2 gained and the Fourier transform infrared spectroscopy figure of vulcabond MDI;
Fig. 2 is the essence Nano capsule of the embodiment of the present invention 3,4 gained and the Fourier transform infrared spectroscopy figure of vulcabond IPDI;
Fig. 3 is the Dynamic light scattering grain size distribution of the essence Nano capsule of the embodiment of the present invention 1;
Fig. 4 is the Dynamic light scattering grain size distribution of the essence Nano capsule of the embodiment of the present invention 2;
Fig. 5 is the Dynamic light scattering grain size distribution of the essence Nano capsule of the embodiment of the present invention 3;
Fig. 6 is the Dynamic light scattering grain size distribution of the essence Nano capsule of the embodiment of the present invention 4;
Fig. 7,8 is electron scanning micrograph figure of the essence Nano capsule of the embodiment of the present invention 1;
Fig. 9,10 is transmission electron microscope photo figure of the essence Nano capsule of the embodiment of the present invention 1;
Figure 11 is the essence Nano capsule of the embodiment of the present invention 1 and the thermal gravimetric analysis curve figure of peppermint essence;
Figure 12 is the essence Nano capsule of the embodiment of the present invention 2 and the thermal gravimetric analysis curve figure of peppermint essence;
Figure 13 is the essence Nano capsule of the embodiment of the present invention 3 and the thermal gravimetric analysis curve figure of peppermint essence;
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Emulsifying agent D-425 of the present invention is purchased from Nanjing Jie Run Science and Technology Ltd..
Embodiment 1
Take polyureas as an essence Nano capsule for cyst wall, be made up of oil phase component and water phase components; Described oil phase component is made up of essence 15wt% and vulcabond 3.2wt%; Described water phase components is made up of emulsifying agent 1.5wt%, diamines 1.44wt% and deionized water 78.86wt%, and the weight percent sum of all components is 100%.Described essence is Peppermint Oil.Described vulcabond is 4,4 '-diphenylmethanediisocyanate MDI.Described emulsifying agent is D-425.Described diamines is hexanediamine HMDA.
The preparation method of above-mentioned with polyureas the is essence Nano capsule of cyst wall is:
(1) preparation of aqueous phase:
Take each oil phase component and water phase components by weight percentage, emulsifying agent D-425 is placed in beaker, adds deionized water, under magnetic stirring apparatus effect, stir 2h, emulsifying agent is dissolved completely, be mixed with the emulsifier aqueous solution that 16.6g concentration is 6wt%, for subsequent use.With the HMDA aqueous solution that deionized water preparation 3.6g concentration is 40wt%; In 100ml beaker, add 16.6g emulsifier aqueous solution, then add remaining 53.2g deionized water, stir, obtain aqueous phase;
(2) preparation of oil phase
In 100ml beaker, add 3.2g vulcabond MDI, then add the mixing of 15g Peppermint Oil, be stirred to and dissolve each other completely, obtained oil phase;
(3) formation of miniemulsion
Under normal temperature, oil phase is joined in aqueous phase, clarifixator is used to carry out emulsification pretreatment 3min with speed 6600rpm, form primary emulsifying emulsion oil-in-water, this emulsion is placed in ultrasonic cell disruptor and carries out ultrasonication 30min, ultrasonic power is 50% (total power is 900W), obtains the o/w miniemulsion after ultrasonic wave dispersion;
(4) formation of Nano capsule
O/w miniemulsion after above-mentioned ultrasonic wave dispersion is placed in constant temperature blender with magnetic force, drip the HMDA aqueous solution that 3.6g concentration is 40wt%, temperature constant magnetic stirring 30min at 35 DEG C, is rapidly heated to 55 DEG C, temperature constant magnetic stirring 2h, is namely able to the essence Nano capsule paste that polyureas is cyst wall.
As is seen in figs 7-10, the pattern of scanning electronic microscope and transmission electron microscope observation microcapsule is ganoid spherical and have obvious nucleocapsid structure; As shown in Figure 3, the particle diameter that Nano capsule analyzed by dynamic/rheological properties instrument is 50 ~ 350nm, and median size is 141.1nm, and polydispersity coefficient PDI mean value is 0.176; As shown in Figure 1, infrared spectra contrast susceptible of proof vulcabond and diamine polymerization reaction generate polyureas, determine the constitutional features of Nano capsule; As shown in figure 11, thermogravimetry shows that Nano capsule has satisfactory stability below 260.3 DEG C.
Embodiment 2
Take polyureas as an essence Nano capsule for cyst wall, be made up of oil phase component and water phase components; Described oil phase component is made up of essence 12wt% and vulcabond 3.2wt%; Described water phase components is made up of emulsifying agent 1.5wt%, diamines 1.44wt% and deionized water 81.86wt%, and the weight percent sum of all components is 100%.Described essence is Peppermint Oil.Described vulcabond is 4,4 '-diphenylmethanediisocyanate MDI.Described emulsifying agent is D-425.Described diamines is hexanediamine HMDA.
The preparation method of above-mentioned with polyureas the is essence Nano capsule of cyst wall is:
(1) preparation of aqueous phase:
Take each oil phase component and water phase components by weight percentage, emulsifying agent D-425 is placed in beaker, adds deionized water, under magnetic stirring apparatus effect, stir 2h, emulsifying agent is dissolved completely, be mixed with the emulsifier aqueous solution that 16.6g concentration is 6wt%, for subsequent use.With the HMDA aqueous solution that deionized water preparation 3.6g concentration is 40wt%; In 100ml beaker, add 16.6g emulsifier aqueous solution, then add remaining 56.2g deionized water, stir, obtain aqueous phase;
(2) preparation of oil phase
In 100ml beaker, add 3.2g vulcabond MDI, then add 12g Peppermint Oil, be stirred to and dissolve each other completely, obtained oil phase;
(3) formation of miniemulsion
Under normal temperature, oil phase is joined in aqueous phase, electric mixer is used to carry out dispersed with stirring emulsification 5min with speed 400rpm, form primary emulsifying emulsion oil-in-water, this emulsion is placed in ultrasonic cell disruptor and carries out ultrasonication 30min, ultrasonic power is 50% (total power is 900W), obtains the o/w miniemulsion after ultrasonic wave dispersion;
(4) formation of Nano capsule
O/w miniemulsion after above-mentioned ultrasonic wave dispersion is placed in constant temperature blender with magnetic force, drip the HMDA aqueous solution that 3.6g concentration is 40wt%, temperature constant magnetic stirring 30min at 35 DEG C, is rapidly heated to 55 DEG C, temperature constant magnetic stirring 2h, is namely able to the essence Nano capsule paste that polyureas is cyst wall.
The pattern of scanning electronic microscope and transmission electron microscope observation microcapsule is ganoid spherical and have obvious nucleocapsid structure; As shown in Figure 4, the particle diameter that Nano capsule analyzed by dynamic/rheological properties instrument is 50 ~ 450nm, and median size is 159.4nm, and polydispersity coefficient PDI mean value is 0.208; As shown in Figure 1, infrared spectra contrast susceptible of proof vulcabond and diamine polymerization reaction generate polyureas, determine the constitutional features of Nano capsule; As shown in figure 12, thermogravimetry shows that Nano capsule has satisfactory stability below 255.7 DEG C.
Embodiment 3
Take polyureas as an essence Nano capsule for cyst wall, be made up of oil phase component and water phase components; Described oil phase component is made up of essence 10wt% and vulcabond 3.2wt%; Described water phase components is made up of emulsifying agent 1.5wt%, diamines 1.44wt% and deionized water 83.86wt%, and the weight percent sum of all components is 100%.Described essence is Peppermint Oil.Described vulcabond is isophorone diisocyanate IPDI.Described emulsifying agent is D-425.Described diamines is hexanediamine HMDA.
The preparation method of above-mentioned with polyureas the is essence Nano capsule of cyst wall is:
(1) preparation of aqueous phase:
Take each oil phase component and water phase components by weight percentage, emulsifying agent D-425 is placed in beaker, adds deionized water, under magnetic stirring apparatus effect, stir 2h, emulsifying agent is dissolved completely, be mixed with the emulsifier aqueous solution that 16.6g concentration is 6wt%, for subsequent use.With the HMDA aqueous solution that deionized water preparation 3.6g concentration is 40wt%; In 100ml beaker, add 16.6g emulsifier aqueous solution, then add remaining 58.2g deionized water, stir, obtain aqueous phase;
(2) preparation of oil phase
In 100ml beaker, add 3.2g vulcabond IPDI, then add 10g Peppermint Oil, be stirred to and dissolve each other completely, obtained oil phase;
(3) formation of miniemulsion
Under normal temperature, oil phase is joined in aqueous phase, electric mixer is used to carry out dispersed with stirring emulsification 5min with speed 1000rpm, form primary emulsifying emulsion oil-in-water, this emulsion is placed in ultrasonic cell disruptor and carries out ultrasonication 30min, ultrasonic power is 50% (total power is 900W), obtains the o/w miniemulsion after ultrasonic wave dispersion;
(4) formation of Nano capsule
O/w miniemulsion after above-mentioned ultrasonic wave dispersion is placed in constant temperature blender with magnetic force, drip the HMDA aqueous solution that 3.6g concentration is 40wt%, temperature constant magnetic stirring 30min at 35 DEG C, is rapidly heated to 55 DEG C, temperature constant magnetic stirring 2h, is namely able to the essence Nano capsule paste that polyureas is cyst wall.
The pattern of scanning electronic microscope and transmission electron microscope observation microcapsule is ganoid spherical and have obvious nucleocapsid structure; As shown in Figure 5, the particle diameter that Nano capsule analyzed by dynamic/rheological properties instrument is 90 ~ 900nm, and median size is 295.95nm, and polydispersity coefficient PDI mean value is 0.260; As shown in Figure 2, infrared spectra contrast susceptible of proof vulcabond and diamine polymerization reaction generate polyureas, determine the constitutional features of Nano capsule; As shown in figure 13, thermogravimetry shows that Nano capsule has satisfactory stability below 304.3 DEG C.
Embodiment 4
Take polyureas as an essence Nano capsule for cyst wall, be made up of oil phase component and water phase components; Described oil phase component is made up of essence 1.5wt% and vulcabond 3.2wt%; Described water phase components is made up of emulsifying agent 1.5wt%, diamines 1.44wt% and deionized water 92.36wt%, and the weight percent sum of all components is 100%.Described essence is Peppermint Oil.Described vulcabond is isophorone diisocyanate IPDI.Described emulsifying agent is D-425.Described diamines is hexanediamine HMDA.
The preparation method of above-mentioned with polyureas the is essence Nano capsule of cyst wall is:
(1) preparation of aqueous phase:
Take each oil phase component and water phase components by weight percentage, emulsifying agent D-425 is placed in beaker, adds deionized water, under magnetic stirring apparatus effect, stir 2h, emulsifying agent is dissolved completely, be mixed with the emulsifier aqueous solution that 16.6g concentration is 6wt%, for subsequent use.With the HMDA aqueous solution that deionized water preparation 3.6g concentration is 40wt%; In 100ml beaker, add 16.6g emulsifier aqueous solution, then add remaining 53.2g deionized water, stir, obtain aqueous phase;
(2) preparation of oil phase
In 100ml beaker, add 3.2g vulcabond IPDI, then add 15g Peppermint Oil, be stirred to and dissolve each other completely, obtained oil phase;
(3) formation of miniemulsion
Under normal temperature, oil phase is joined in aqueous phase, clarifixator is used to carry out emulsification pretreatment 3min with speed 6600rpm, form primary emulsifying emulsion oil-in-water, this emulsion is placed in ultrasonic cell disruptor and carries out ultrasonication 30min, ultrasonic power is 50% (total power is 900W), obtains the o/w miniemulsion after ultrasonic wave dispersion;
(4) formation of Nano capsule
O/w miniemulsion after above-mentioned ultrasonic wave dispersion is placed in constant temperature blender with magnetic force, drip the HMDA aqueous solution that 3.6g concentration is 40wt%, temperature constant magnetic stirring 30min at 35 DEG C, is rapidly heated to 55 DEG C, temperature constant magnetic stirring 2h, is namely able to the essence Nano capsule paste that polyureas is cyst wall.
The pattern of scanning electronic microscope and transmission electron microscope observation microcapsule is ganoid spherical and have obvious nucleocapsid structure; As shown in Figure 6, the particle diameter that microcapsule analyzed by dynamic/rheological properties instrument is 80 ~ 900nm, and median size is 289.55nm, and polydispersity coefficient PDI mean value is 0.275; As shown in Figure 2, infrared spectra contrast susceptible of proof vulcabond and diamine polymerization reaction generate polyureas, determine the constitutional features of Nano capsule; Thermogravimetry shows that Nano capsule has satisfactory stability below 304.3 DEG C.
Claims (8)
1. be an essence Nano capsule for cyst wall with polyureas, it is characterized in that, be made up of oil phase component and water phase components; Described oil phase component is made up of essence 5.0 ~ 20.0wt% and vulcabond 2.5 ~ 4.5wt%; Described water phase components is made up of emulsifying agent 0.5 ~ 5.0wt%, diamines 0.5 ~ 2.5wt% and deionized water 68.0 ~ 91.5wt%, and the weight percent sum of all components is 100%.
2. be the essence Nano capsule of cyst wall as claimed in claim 1 with polyureas, it is characterized in that, described essence is Peppermint Oil.
3. as claimed in claim 1 take polyureas as the essence Nano capsule of cyst wall, and it is characterized in that, described vulcabond is 4, one or both in 4 '-diphenylmethanediisocyanate and isophorone diisocyanate.
4. be the essence Nano capsule of cyst wall as claimed in claim 1 with polyureas, it is characterized in that, described emulsifying agent is D-425.
5. be the essence Nano capsule of cyst wall as claimed in claim 1 with polyureas, it is characterized in that, described diamines is 1,6-hexane diamines.
6. according to any one of claim 1-5 take polyureas as the preparation method of the essence Nano capsule of cyst wall, it is characterized in that, comprising:
Step 1: take each oil phase component and water phase components by weight percentage, preparation mass percent concentration is 2
-the emulsifier aqueous solution of 20%; Compound concentration is 8 ~ 40wt% bis-amine aqueous solution; By emulsifier aqueous solution and the mixing of remaining deionized water, obtain aqueous phase;
Step 2: by vulcabond and essence mixing, be stirred to and dissolve each other completely, obtained oil phase;
Step 3: under normal temperature, the oil phase of step 2 gained is joined in the aqueous phase of step 1 gained, clarifixator or homogenizer is used to carry out emulsification 3 ~ 5min, obtain primary emulsifying o/w emulsion, this emulsion is placed in ultrasonic cell disruptor and carries out ultrasonication, obtain the o/w emulsion after ultrasonic wave dispersion;
Step 4: the o/w emulsion after above-mentioned ultrasonic wave dispersion is placed in constant temperature blender with magnetic force, two amine aqueous solutions of preparation in step 1 are dripped under 30 ~ 40 DEG C of water-baths, heat up after constant temperature 20 ~ 30min, constant temperature 1.5 ~ 2.5h at 50 ~ 60 DEG C, is namely able to the essence Nano capsule that polyureas is cyst wall.
7. be the preparation method of the essence Nano capsule of cyst wall as claimed in claim 6 with polyureas, it is characterized in that, when the use clarifixator in described step 3 carries out emulsification, shearing rate is 4000 ~ 9000rpm.
8. be the preparation method of the essence Nano capsule of cyst wall as claimed in claim 6 with polyureas, it is characterized in that, the ultrasonic time in described step 3 is 20min ~ 40min, and ultrasonic power is 30% ~ 60%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510030379.5A CN104593151A (en) | 2015-01-21 | 2015-01-21 | Essence nanocapsule taking polyurea as capsule wall and preparation method of essence nanocapsule |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510030379.5A CN104593151A (en) | 2015-01-21 | 2015-01-21 | Essence nanocapsule taking polyurea as capsule wall and preparation method of essence nanocapsule |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104593151A true CN104593151A (en) | 2015-05-06 |
Family
ID=53119211
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510030379.5A Pending CN104593151A (en) | 2015-01-21 | 2015-01-21 | Essence nanocapsule taking polyurea as capsule wall and preparation method of essence nanocapsule |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104593151A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107602852A (en) * | 2017-08-18 | 2018-01-19 | 浙江大学 | A kind of polymer support for carried perfume, preceding fragrant body and its preparation method and application |
| CN108579634A (en) * | 2018-04-13 | 2018-09-28 | 天津工业大学 | A kind of preparation method of hydrophobic amine capsule |
| CN109526952A (en) * | 2018-12-28 | 2019-03-29 | 山东农业大学 | A kind of glycosylated pesticide nano micro-capsule and preparation method thereof |
| CN109923144A (en) * | 2016-11-07 | 2019-06-21 | 湛新荷兰有限公司 | The method for preparing thixotropic composition |
| CN112716029A (en) * | 2020-12-21 | 2021-04-30 | 安徽中烟工业有限责任公司 | Granular nano-microcapsule for heating cigarettes and preparation method thereof |
| CN113019272A (en) * | 2021-03-12 | 2021-06-25 | 东莞波顿香料有限公司 | Essence capsule, preparation method thereof and washing and caring product |
| CN113122282A (en) * | 2019-12-30 | 2021-07-16 | 江苏集萃智能液晶科技有限公司 | Temperature-sensitive chromogenic liquid crystal microcapsule, preparation method thereof and temperature-sensitive chromogenic container |
| CN113893793A (en) * | 2021-10-25 | 2022-01-07 | 浙江大学 | Size-controllable flexible ionic liquid nano microcapsule and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1057755A (en) * | 1990-06-25 | 1992-01-15 | 高韵苕 | The encystation method of essence microcapsule |
| WO2004098767A1 (en) * | 2003-05-11 | 2004-11-18 | Ben Gurion University Of The Negev Research And Development Authority | Encapsulated essential oils |
-
2015
- 2015-01-21 CN CN201510030379.5A patent/CN104593151A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1057755A (en) * | 1990-06-25 | 1992-01-15 | 高韵苕 | The encystation method of essence microcapsule |
| WO2004098767A1 (en) * | 2003-05-11 | 2004-11-18 | Ben Gurion University Of The Negev Research And Development Authority | Encapsulated essential oils |
Non-Patent Citations (2)
| Title |
|---|
| 曾戎等编著: "《生物医用仿生高分子材料》", 31 October 2010, 华南理工大学出版社 * |
| 朱珠等主编: "《食品工艺学概论》", 31 March 2014, 郑州大学出版社 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109923144A (en) * | 2016-11-07 | 2019-06-21 | 湛新荷兰有限公司 | The method for preparing thixotropic composition |
| CN107602852A (en) * | 2017-08-18 | 2018-01-19 | 浙江大学 | A kind of polymer support for carried perfume, preceding fragrant body and its preparation method and application |
| CN108579634A (en) * | 2018-04-13 | 2018-09-28 | 天津工业大学 | A kind of preparation method of hydrophobic amine capsule |
| CN108579634B (en) * | 2018-04-13 | 2020-11-20 | 天津工业大学 | Preparation method of hydrophobic amine capsule |
| CN109526952A (en) * | 2018-12-28 | 2019-03-29 | 山东农业大学 | A kind of glycosylated pesticide nano micro-capsule and preparation method thereof |
| CN109526952B (en) * | 2018-12-28 | 2021-12-17 | 山东农业大学 | Glycosylated pesticide nano microcapsule and preparation method thereof |
| CN113122282A (en) * | 2019-12-30 | 2021-07-16 | 江苏集萃智能液晶科技有限公司 | Temperature-sensitive chromogenic liquid crystal microcapsule, preparation method thereof and temperature-sensitive chromogenic container |
| CN113122282B (en) * | 2019-12-30 | 2023-03-21 | 江苏集萃智能液晶科技有限公司 | Temperature-sensitive chromogenic liquid crystal microcapsule, preparation method thereof and temperature-sensitive chromogenic container |
| CN112716029A (en) * | 2020-12-21 | 2021-04-30 | 安徽中烟工业有限责任公司 | Granular nano-microcapsule for heating cigarettes and preparation method thereof |
| CN113019272A (en) * | 2021-03-12 | 2021-06-25 | 东莞波顿香料有限公司 | Essence capsule, preparation method thereof and washing and caring product |
| CN113893793A (en) * | 2021-10-25 | 2022-01-07 | 浙江大学 | Size-controllable flexible ionic liquid nano microcapsule and preparation method and application thereof |
| CN113893793B (en) * | 2021-10-25 | 2022-12-09 | 浙江大学 | Size-controllable flexible ionic liquid nano microcapsule and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104593151A (en) | Essence nanocapsule taking polyurea as capsule wall and preparation method of essence nanocapsule | |
| CN111225718B (en) | Hydrogel beads | |
| EP2793800A1 (en) | Improvements in or relating to the encapsulation of perfumes | |
| WO2006010088A1 (en) | Method for providing customized products | |
| CN105112181A (en) | Functional plant essential oil handmade soap and preparation method thereof | |
| CA2501014A1 (en) | Emulsifier | |
| CN107252400A (en) | Vegetable fat nanoemulsions prepared by a kind of use D phases emulsion process and preparation method thereof | |
| EP2870192B1 (en) | Water-dispersible polyamide powder | |
| TW200916120A (en) | Deodorant compositions | |
| EA025197B1 (en) | Highly concentrated, spherical biopolymer gel particle suspensions prepared by hipe-gelation process | |
| EP3337452B1 (en) | Encapsulated lactams | |
| CN107137714A (en) | Blumea balsamifera essence oil nanometer microcapsules, its preparation method and its application | |
| CN107106466A (en) | Include the stabilising dispersions of aromatic drop | |
| Zheng et al. | Natural rheological modifiers for personal care | |
| CN104312540A (en) | A green phase change microcapsule with mint fragrance and a preparing method thereof | |
| EP3668602A1 (en) | Microcapsules with improved deposition | |
| WO2012001299A1 (en) | Cosmetic composition containing copa | |
| CN104841343A (en) | Preparation method for fragrant microcapsule and silver-loaded multilayered microcapsule emulsion thereof | |
| CN104651055A (en) | Polyurea microcapsule with aromatic smell and preparation method of polyurea microcapsule | |
| JP5809956B2 (en) | Method for producing hydrogel particles | |
| Gao et al. | Unexpected rheological behavior of a hydrophobic associative shellac-based oligomeric food thickener | |
| CN104693774A (en) | Polyethyleneglycol diacrylate aquagel with aromatic odor and preparation method thereof | |
| CN102256694B (en) | Method for producing hydrogel particles | |
| KR101654576B1 (en) | Nanoemulsion containing high content of hydrophobic ingredients and the method for preparing thereof | |
| JP6121887B2 (en) | Spray-type cosmetics |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150506 |