CN103432970A - Method for preparing organic-inorganic composite microcapsule through complex coacervation - Google Patents
Method for preparing organic-inorganic composite microcapsule through complex coacervation Download PDFInfo
- Publication number
- CN103432970A CN103432970A CN2013103894463A CN201310389446A CN103432970A CN 103432970 A CN103432970 A CN 103432970A CN 2013103894463 A CN2013103894463 A CN 2013103894463A CN 201310389446 A CN201310389446 A CN 201310389446A CN 103432970 A CN103432970 A CN 103432970A
- Authority
- CN
- China
- Prior art keywords
- micro
- capsule
- organic
- wall material
- solution
- 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
Images
Landscapes
- Manufacturing Of Micro-Capsules (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses a method for preparing an organic-inorganic composite microcapsule through complex coacervation, which relates to a method for preparing a microcapsule through complex coacervation and aims at solving the problems of poor volatilization resistance and low encapsulation efficiency of a core material of the existing composite microcapsule. The preparation method comprises the steps of: (1) dissolving an anionic-macromolecule or amphoteric natural-macromolecule wall material in water to form a solution A; (2) dissolving a cationic-macromolecule or amphoteric natural-macromolecule wall material in water to form a solution B; (3) adding a capsule core material in the solution A, and performing high shearing, emulsification and homogenization; (4) adding O/W (oil/water-phase) emulsion in the solution B and stirring at constant temperature to obtain a mixed solution; (5) adjusting the pH value of the mixed solution and adding water to dilute the mixed solution; (6) adding inorganic nanoparticles, reducing the temperature, adding a curing agent, adding a polyvinyl alcohol solution, and performing leaching and washing, thereby obtaining the organic-inorganic composite microcapsule. The composite microcapsule obtained by the method has high volatilization resistance and 92% of encapsulation efficiency and is mainly used in the fields of foods, medicines, cosmetics and bioengineering.
Description
Technical field
The present invention relates to the method for the standby micro-capsule of a kind of multiple coacervation legal system.
Background technology
The organic and inorganic composite microcapsule is the emerging field of macromolecule subject.Usually organic-inorganic structure the compound particle of preparation adopts emulsion polymerization mostly.At first emulsion polymerization is that silica is carried out to amination, and the rear water of directly putting into, add monomer and initator to carry out emulsion polymerisation, directly is coated on inorganic nano-particle and forms nano particle, take inorganic nano-particle silica as the template core.The patent that is called " method for preparing inorganic-organic hybridization nano microcapsule that the polymer of take is core " as Chinese patent CN1669629 name is with vinyl monomer emulsion polymerisation synthetic polymer seed, with the siloxanyl monomers copolymerization, obtain hybrid inorganic-organic type core-shell latex particles again.Perhaps by adding surfactant to reduce surface of inorganic particles polarity, improve the compatibility between itself and macromolecule, strengthen covered effect.It is masterplate with organic molecule hydrocarbon drop that Chinese patent CN1680014 name is called " method for preparing inorganic-organic hybridization nano microcapsule that the organic molecule hydrocarbon of take is template " record, adopt the mini-emulsion polymerization method, with vinyl monomer and siloxanyl monomers condensation.Also there is the layer-by-layer of employing to build self-assembled multilayer film on Colloidal Nanosize Silica Template and prepare microcapsules, as the document of the people such as Li Dong " Paper Science & Technology " the 3rd phase in 2012 " utilizes nanometer SiO
2template prepares the research of chitosan quaternary ammonium salt/sodium alginate self assembly microcapsules " in put down in writing the natural macromolecular material application layer-by-layer that adopts opposite charges and prepare and take the microballoon that silica is capsule-core.
The document of prior art is found, the document " preparation of thermo-sensitive material microcapsules and temperature sensitive ink " of the people such as Zhang Yuxi in June calendar year 2001 " fine chemistry industry ", its preparation method is to add silica as interleaving agent in the gelatin-gum arabic micro-capsule completed in preparation, but the document is that the silica added after solidifying is to play the effect that prevents the micro-capsule adhesion.The people such as Spomenka Simovic are at Journal of Controlled Release, 143 (3), 2010, prepare silica-grease mixing micro-capsule in 367 – 373 " An oral delivery system for indomethicin engineered from cationic lipid emulsions and silica nanoparticles ", that silica first is mixed into to capsule-core with oil, coated, silica wherein only plays adsorbent.
Summary of the invention
The present invention seeks to the poor and low problem of envelop rate of the anti-volatile performance of core materials in order to solve existing composite microcapsule, and the method for the organic-inorganic compounding micro-capsule that provides a kind of complex coacervation to prepare.
The method of organic-inorganic compounding micro-capsule prepared by complex coacervation of the present invention follows these steps to realize:
One, the wall material A of anionic macromolecule or both sexes natural polymer is added to the water, after placing 7～10 hours natural swellings, is heated to 70～90 ℃ and wall material A is dissolved fully form the solution A that solid content is 1%～40%;
Two, the wall material B of cationic high-molecular or both sexes natural polymer is added to the water, after placing 7～10 hours natural swellings, is heated to 40～60 ℃ and wall material B is dissolved fully form the solution B that solid content is 0.1%～40%;
Three, oiliness or oil-soluble core-clad material are joined in the solution A of step 1, then put into mulser emulsification 30～50s, then be placed in the homogenizer homogeneous 3～5 times, obtain O/W emulsion;
Four, O/W emulsion step 3 obtained is added drop-wise in solution B, at 40～60 ℃ of lower constant temperature, stirs, and obtains mixed liquor;
Five, add acidity regulator in the mixed liquor in step 4, be adjusted to pH of mixed=4, and then be diluted with water 1～2 times, obtain the micro-capsule suspension after stirring;
Six, add the inorganic nano-particle that accounts for wall material A and wall material B gross mass 1%～30% in the micro-capsule suspension, add again curing agent after being cooled to 8～11 ℃, solidify 1～6h, then adding poly-vinyl alcohol solution to make polyvinyl alcohol mass concentration in system is 0.8%～1.2%, micro-capsule suspension after reaction 1～2h is solidified, collect micro-capsule after micro-capsule suspension suction filtration, micro-capsule, through water washing 1～3 time, obtains the organic and inorganic composite microcapsule after drying;
Wherein said wall material A is Arabic gum, xanthans, sodium carboxymethylcellulose, sodium alginate or protein, and wall material B is shitosan, gelatin or protein;
Described curing agent is TG enzyme, glutaraldehyde, formaldehyde or Geniposide.
A kind of organic and inorganic composite microcapsule of the present invention is to using oiliness or oil-soluble core-clad material as core, take the multiple condensate of cross-linked polymer that wall material A and wall material B form and inorganic nano-particle is wrapped up core as the capsule material, make the multiple condensate curing cross-linked of macromolecule by curing agent, and inorganic nano-particle is adsorbed in the network structure of the multiple condensate of cross-linked polymer; Its mesospore material A is Arabic gum, xanthans, sodium carboxymethylcellulose, sodium alginate or protein, and wall material B is shitosan, gelatin or protein, and curing agent is TG enzyme, glutaraldehyde, formaldehyde or Geniposide.
The organic and inorganic composite microcapsule that the present invention adopts complex coacervation to prepare comprises following advantage:
1, the organic and inorganic composite microcapsule has good anti-volatile performance.By with the easy oxidation core of embedding treatment not, to carry out accelerated oxidation experiment contrast known, core menthol raw material in the organic and inorganic composite microcapsule accelerates 3 days only oxidized 9.8% under 60 ℃, and under equal conditions not the menthol of microencapsulation under 60 ℃, accelerate 3 days oxidized 60%, and then demonstrate the anti-volatile performance that the organic and inorganic composite microcapsule is good.
2, the present invention is prepared into micro-capsule by core, can control the rate of release of core, improves its bioavilability.
3, add poly-vinyl alcohol solution can prevent the core diffusional precipitation after solidifying in the preparation process of complex coacervation, also can make micro-capsule be uniformly dispersed, adhesion.
4, the envelop rate of the organic and inorganic composite microcapsule of preparation reaches as high as 92%, the medicine carrying amount reaches as high as 70%, due to core by the effective embedding of wall material, effective prevention itself and other material generation redox reaction, conveniently with other medicines, mix interpolation, and the preparation process simple economy, be easy to suitability for industrialized production, be mainly used in food, medicine, cosmetics and bioengineering field.
The accompanying drawing explanation
Fig. 1 is the investigation figure of the anti-volatile performance of organic and inorganic composite microcapsule that obtains of embodiment mono-, ◆ mean the menthol after microencapsulation, ■ means the menthol of not microencapsulation;
Fig. 2 is the laser particle distribution map of the organic and inorganic composite microcapsule that obtains of embodiment mono-, and the ordinate of particle diameter distribution map is volume cumulative percentage q
2/ Δ ㏒
x, wherein X is particle diameter, q
2for the cross-check multiple correlation coefficient;
Fig. 3 is the Electronic Speculum figure of the organic and inorganic composite microcapsule that obtains of embodiment mono-.
The specific embodiment
The specific embodiment one: the method that the present embodiment complex coacervation prepares organic-inorganic compounding micro-capsule follows these steps to implement:
One, the wall material A of anionic macromolecule or both sexes natural polymer is added to the water, after placing 7～10 hours natural swellings, is heated to 70～90 ℃ and wall material A is dissolved fully form the solution A that solid content is 1%～40%;
Two, the wall material B of cationic high-molecular or both sexes natural polymer is added to the water, after placing 7～10 hours natural swellings, is heated to 40～60 ℃ and wall material B is dissolved fully form the solution B that solid content is 0.1%～40%;
Three, oiliness or oil-soluble core-clad material are joined in the solution A of step 1, then put into mulser emulsification 30～50s, then be placed in the homogenizer homogeneous 3～5 times, obtain O/W emulsion;
Four, O/W emulsion step 3 obtained is added drop-wise in solution B, at 40～60 ℃ of lower constant temperature, stirs, and obtains mixed liquor;
Five, add acidity regulator in the mixed liquor in step 4, be adjusted to pH of mixed=4, and then be diluted with water 1～2 times, obtain the micro-capsule suspension after stirring;
Six, add the inorganic nano-particle that accounts for wall material A and wall material B gross mass 1%～30% in the micro-capsule suspension, add again curing agent after being cooled to 8～11 ℃, solidify 1～6h, then adding poly-vinyl alcohol solution to make polyvinyl alcohol mass concentration in system is 0.8%～1.2%, micro-capsule suspension after reaction 1～2h is solidified, collect micro-capsule after micro-capsule suspension suction filtration, micro-capsule, through water washing 1～3 time, obtains the organic and inorganic composite microcapsule after drying;
Wherein said wall material A is Arabic gum, xanthans, sodium carboxymethylcellulose, sodium alginate or protein, and wall material B is shitosan, gelatin or protein; Described curing agent is TG enzyme, glutaraldehyde, formaldehyde or Geniposide.
It is to using oiliness or oil soluble material as core that present embodiment adopts organic and inorganic composite microcapsule that complex coacervation prepares, take the multiple condensate of cross-linked polymer that wall material A and wall material B form and inorganic nano-particle is wrapped up core as the capsule material, make the multiple condensate curing cross-linked of macromolecule by curing agent, inorganic nano-particle is adsorbed on cross-linked polymer multiple condensate surface or is embedded in the network structure of the multiple condensate of macromolecule.The organic and inorganic composite microcapsule particle diameter obtained is evenly distributed, and average grain diameter is about the 500nm left and right, good to the anti-volatile performance of oiliness or oil-soluble core, and envelop rate can reach more than 90%.
The specific embodiment two: present embodiment is different from the specific embodiment one is that core-clad material in step 3 is menthol, Angelica oil or eugenol.Other step and parameter are identical with the specific embodiment one.
The specific embodiment three: what present embodiment was different from the specific embodiment one or two is that step 3 is put into the rotating speed emulsification of mulser with 10000r/min.Other step and parameter are identical with the specific embodiment one or two.
The specific embodiment four: present embodiment is different from one of specific embodiment one to three is that mixing speed during step 4 constant temperature stirs is 800～1000r/min.Other step and parameter are identical with one of specific embodiment one to three.
The specific embodiment five: present embodiment is different from one of specific embodiment one to four is that acidity regulator in step 5 is hydrochloric acid, acetic acid or phosphoric acid.Other step and parameter are identical with one of specific embodiment one to four.
The specific embodiment six: present embodiment is different from one of specific embodiment one to five is that inorganic nano-particle in step 6 is silica, titanium dioxide, Magnesiumaluminumsilicate, talcum powder, dolomol or superfine silica gel powder.Other step and parameter are identical with one of specific embodiment one to five.
The specific embodiment seven: present embodiment is different from one of specific embodiment one to six be the step 6 micro-capsule through water washing, drying, drying means is drying under reduced pressure.Other step and parameter are identical with one of specific embodiment one to six.
The specific embodiment eight: what present embodiment was different from one of specific embodiment one to seven is that wall material A is Arabic gum, and wall material B is gelatin, and curing agent is the TG enzyme.Other step and parameter are identical with one of specific embodiment one to seven.
Embodiment mono-: the method that the present embodiment complex coacervation prepares organic-inorganic compounding micro-capsule follows these steps to realize:
One, 0.4g wall material A is added in 20ml water, after placing 8 hours natural swellings, be heated to 80 ℃ and make wall material A dissolve the formation solution A fully;
Two, 0.4g wall material B is added in 20ml water, after placing 8 hours natural swellings, be heated to 50 ℃ and make wall material B dissolve the formation solution B fully;
Three, the 0.4g menthol is dissolved in the 4ml chloroform, the chloroform soln that is dissolved with menthol joins in the solution A of step 1 as core-clad material, put into again the rotating speed emulsification 50s of mulser with 10000r/min, then be placed in the homogenizer homogeneous 3 times, obtain O/W emulsion;
Four, O/W emulsion step 3 obtained is added drop-wise in solution B, at 50 ℃ of lower constant temperature, stirs, and obtains mixed liquor;
Five, add acetic acid in the mixed liquor in step 4, be adjusted to pH of mixed=4, and then be diluted with water 1 times, obtain the micro-capsule suspension after stirring;
Six, to the silica that adds 0.1g in the micro-capsule suspension, be cooled to the TG enzyme that adds again 0.7g after 9 ℃, solidify 1h, then adding poly-vinyl alcohol solution to make polyvinyl alcohol mass concentration in system is 1%, micro-capsule suspension after reaction 1h is solidified, collect micro-capsule after micro-capsule suspension suction filtration, micro-capsule, through water washing 3 times, obtains the organic and inorganic composite microcapsule after drying;
Its mesospore material A is Arabic gum, and wall material B is gelatin; Mixing speed during step 4 constant temperature stirs is 1000r/min.
It is 10% that the present embodiment step 4 adds the concentration of acetic acid; Step 5 is diluted with water 1 times, and wherein water temperature is 50 ℃; The step 6 micro-capsule is through water washing, drying, and wherein drying is at 40 ℃ of lower drying under reduced pressure.The organic and inorganic composite microcapsule good fluidity that preparation method by the present embodiment obtains, uniform particle diameter, envelop rate can reach 92.3%.From the known menthol of investigation figure (Fig. 1) of the anti-volatile performance of organic and inorganic composite microcapsule, after microencapsulation, under 60 ℃, accelerate 3 days, only oxidized 9.8%, and the menthol of microencapsulation under the same conditions oxidized 60% not.
The average grain diameter of the organic and inorganic composite microcapsule that the present embodiment obtains as shown in Figure 2 is about 500nm, and a footpath is evenly distributed.
Embodiment bis-: the method that the present embodiment complex coacervation prepares organic-inorganic compounding micro-capsule follows these steps to realize:
One, 0.4g wall material A is added in 20ml water, after placing 8 hours natural swellings, be heated to 80 ℃ and make wall material A dissolve the formation solution A fully;
Two, 0.4g wall material B is added in 20ml water, after placing 8 hours natural swellings, be heated to 50 ℃ and make wall material B dissolve the formation solution B fully;
Three, join the 0.4g Angelica oil as core-clad material in the solution A of step 1, then put into the rotating speed emulsification 30s of mulser with 10000r/min, then be placed in the homogenizer homogeneous 3 times, obtain O/W emulsion;
Four, O/W emulsion step 3 obtained is added drop-wise in solution B, at 50 ℃ of lower constant temperature, stirs, and obtains mixed liquor;
Five, add acetic acid in the mixed liquor in step 4, be adjusted to pH of mixed=4, and then be diluted with water 1 times, obtain the micro-capsule suspension after stirring;
Six, to the silica that adds 0.1g in the micro-capsule suspension, be cooled to the TG enzyme that adds again 0.7g after 9 ℃, solidify 6h, then adding poly-vinyl alcohol solution to make polyvinyl alcohol mass concentration in system is 1%, micro-capsule suspension after reaction 1h is solidified, collect micro-capsule after micro-capsule suspension suction filtration, micro-capsule, through water washing 2 times, obtains the organic and inorganic composite microcapsule after drying;
Its mesospore material A is for being Arabic gum, and wall material B is gelatin; Mixing speed during step 4 constant temperature stirs is 1000r/min.
It is 10% that the present embodiment step 4 adds the concentration of acetic acid; Step 5 is diluted with water 1 times, and wherein water temperature is 50 ℃; The step 6 micro-capsule is through water washing, drying, and wherein drying is at 40 ℃ of lower drying under reduced pressure.The organic and inorganic composite microcapsule obtained is micro-yellow powder, good fluidity, and uniform particle diameter, envelop rate can reach 90.1%.Angelica oil accelerates 1 day after microencapsulation under 60 ℃, only oxidized 6.4%, and the Angelica oil of microencapsulation under the same conditions oxidized 35% not.
Embodiment tri-: the method that the present embodiment complex coacervation prepares organic-inorganic compounding micro-capsule follows these steps to realize:
One, 0.4g wall material A is added in 20ml water, after placing 8 hours natural swellings, be heated to 80 ℃ and make wall material A dissolve the formation solution A fully;
Two, 0.4g wall material B is added in 20ml water, after placing 8 hours natural swellings, be heated to 50 ℃ and make wall material B dissolve the formation solution B fully;
Three, join the 0.4g eugenol as core-clad material in the solution A of step 1, then put into the rotating speed emulsification 30s of mulser with 10000r/min, then be placed in the homogenizer homogeneous 3 times, obtain O/W emulsion;
Four, O/W emulsion step 3 obtained is added drop-wise in solution B, at 50 ℃ of lower constant temperature, stirs, and obtains mixed liquor;
Five, add acetic acid in the mixed liquor in step 4, be adjusted to pH of mixed=4, and then be diluted with water 1 times, obtain the micro-capsule suspension after stirring;
Six, to the silica that adds 0.1g in the micro-capsule suspension, be cooled to the glutaraldehyde that adds again 0.7g after 9 ℃, solidify 1h, then adding poly-vinyl alcohol solution to make polyvinyl alcohol mass concentration in system is 1%, micro-capsule suspension after reaction 1h is solidified, collect micro-capsule after micro-capsule suspension suction filtration, micro-capsule, through water washing 3 times, obtains the organic and inorganic composite microcapsule after drying;
Its mesospore material A is Arabic gum, and wall material B is gelatin; Mixing speed during step 4 constant temperature stirs is 1000r/min.
It is 10% that the present embodiment step 4 adds the concentration of acetic acid; Step 5 is diluted with water 1 times, and wherein water temperature is 50 ℃; The step 6 micro-capsule is through water washing, drying, and wherein drying is at 40 ℃ of lower drying under reduced pressure.The organic and inorganic composite microcapsule obtained is micro-yellow powder, good fluidity, and uniform particle diameter, envelop rate can reach 90.4%.Eugenol accelerates 1 day after microencapsulation under 60 ℃, only oxidized 8.4%, and the eugenol of microencapsulation under the same conditions oxidized 76% not.
Embodiment tetra-: the method that the present embodiment complex coacervation prepares organic-inorganic compounding micro-capsule follows these steps to realize:
One, 0.4g wall material A is added in 20ml water, after placing 8 hours natural swellings, be heated to 80 ℃ and make wall material A dissolve the formation solution A fully;
Two, 0.4g wall material B is added in 20ml water, after placing 8 hours natural swellings, be heated to 50 ℃ and make wall material B dissolve the formation solution B fully;
Three, the 0.4g Paeonol is dissolved in the 10ml chloroform, the chloroform soln that is dissolved with Paeonol joins in the solution A of step 1 as core-clad material, put into again the rotating speed emulsification 30s of mulser with 10000r/min, then be placed in the homogenizer homogeneous 3 times, obtain O/W emulsion;
Four, O/W emulsion step 3 obtained is added drop-wise in solution B, at 50 ℃ of lower constant temperature, stirs, and obtains mixed liquor;
Five, add acetic acid in the mixed liquor in step 4, be adjusted to pH of mixed=4, and then be diluted with water 1 times, obtain the micro-capsule suspension after stirring;
Six, to the silica that adds 0.1g in the micro-capsule suspension, be cooled to the Geniposide that adds again 0.7g after 9 ℃, solidify 1h, then adding poly-vinyl alcohol solution to make polyvinyl alcohol mass concentration in system is 1%, micro-capsule suspension after reaction 1h is solidified, collect micro-capsule after micro-capsule suspension suction filtration, micro-capsule, through water washing 3 times, obtains the organic and inorganic composite microcapsule after drying;
Its mesospore material A is Arabic gum, and wall material B is gelatin; Mixing speed during step 4 constant temperature stirs is 1000r/min.
It is 10% that the present embodiment step 4 adds the concentration of acetic acid; Step 5 is diluted with water 1 times, and wherein water temperature is 50 ℃; The step 6 micro-capsule is through water washing, drying, and wherein drying is at 40 ℃ of lower drying under reduced pressure.The organic and inorganic composite microcapsule obtained is micro-yellow powder, good fluidity, and uniform particle diameter, envelop rate can reach 90.7%.Paeonol accelerates 1 day after microencapsulation under 60 ℃, only oxidized 7.7%, and the Paeonol of microencapsulation under the same conditions oxidized 75% not.
Claims (8)
1. a complex coacervation prepares the method for organic-inorganic compounding micro-capsule, and the method for the organic-inorganic compounding micro-capsule that it is characterized in that prepared by complex coacervation follows these steps to realize:
One, the wall material A of anionic macromolecule or both sexes natural polymer is added to the water, after placing 7～10 hours natural swellings, is heated to 70～90 ℃ and wall material A is dissolved fully form the solution A that solid content is 1%～40%;
Two, the wall material B of cationic high-molecular or both sexes natural polymer is added to the water, after placing 7～10 hours natural swellings, is heated to 40～60 ℃ and wall material B is dissolved fully form the solution B that solid content is 0.1%～40%;
Three, oiliness or oil-soluble core-clad material are joined in the solution A of step 1, then put into mulser emulsification 30～50s, then be placed in the homogenizer homogeneous 3～5 times, obtain O/W emulsion;
Four, O/W emulsion step 3 obtained is added drop-wise in solution B, at 40～60 ℃ of lower constant temperature, stirs, and obtains mixed liquor;
Five, add acidity regulator in the mixed liquor in step 4, be adjusted to pH of mixed=4, and then be diluted with water 1～2 times, obtain the micro-capsule suspension after stirring;
Six, add the inorganic nano-particle that accounts for wall material A and wall material B gross mass 1%～30% in the micro-capsule suspension, add again curing agent after being cooled to 8～11 ℃, solidify 1～6h, then adding poly-vinyl alcohol solution to make polyvinyl alcohol mass concentration in system is 0.8%～1.2%, micro-capsule suspension after reaction 1～2h is solidified, collect micro-capsule after micro-capsule suspension suction filtration, micro-capsule, through water washing 1～3 time, obtains the organic and inorganic composite microcapsule after drying;
Wherein said wall material A is Arabic gum, xanthans, sodium carboxymethylcellulose, sodium alginate or protein, and wall material B is shitosan, gelatin or protein; Described curing agent is TG enzyme, glutaraldehyde, formaldehyde or Geniposide.
2. a kind of complex coacervation according to claim 1 prepares the method for organic-inorganic compounding micro-capsule, it is characterized in that the core-clad material in step 3 is menthol, Angelica oil or eugenol.
3. a kind of complex coacervation according to claim 1 and 2 prepares the method for organic-inorganic compounding micro-capsule, it is characterized in that step 3 puts into the rotating speed emulsification of mulser with 10000r/min.
4. a kind of complex coacervation according to claim 1 and 2 prepares the method for organic-inorganic compounding micro-capsule, it is characterized in that the mixing speed in the stirring of step 4 constant temperature is 800～1000r/min.
5. a kind of complex coacervation according to claim 1 and 2 prepares the method for organic-inorganic compounding micro-capsule, it is characterized in that the acidity regulator in step 5 is hydrochloric acid, acetic acid or phosphoric acid.
6. a kind of complex coacervation according to claim 1 and 2 prepares the method for organic-inorganic compounding micro-capsule, it is characterized in that the inorganic nano-particle in step 6 is silica, titanium dioxide, Magnesiumaluminumsilicate, talcum powder, dolomol or superfine silica gel powder.
7. a kind of complex coacervation according to claim 1 and 2 prepares the method for organic-inorganic compounding micro-capsule, it is characterized in that the step 6 micro-capsule is through water washing, drying, and drying means is drying under reduced pressure.
8. a kind of complex coacervation according to claim 1 and 2 prepares the method for organic-inorganic compounding micro-capsule, it is characterized in that wall material A is Arabic gum, and wall material B is gelatin, and curing agent is the TG enzyme.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013103894463A CN103432970A (en) | 2013-08-30 | 2013-08-30 | Method for preparing organic-inorganic composite microcapsule through complex coacervation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013103894463A CN103432970A (en) | 2013-08-30 | 2013-08-30 | Method for preparing organic-inorganic composite microcapsule through complex coacervation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103432970A true CN103432970A (en) | 2013-12-11 |
Family
ID=49686739
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013103894463A Pending CN103432970A (en) | 2013-08-30 | 2013-08-30 | Method for preparing organic-inorganic composite microcapsule through complex coacervation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103432970A (en) |
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103876242A (en) * | 2014-04-01 | 2014-06-25 | 广东工业大学 | Microcapsule capable of resisting food-borne pathogenic bacteria as well as preparation method and application thereof |
| CN104496264A (en) * | 2014-12-22 | 2015-04-08 | 江西农业大学 | Method for preparing dry powder organic silicon water repellent microcapsules |
| CN106035739A (en) * | 2016-05-23 | 2016-10-26 | 中国农业大学 | Layer-by-layer self-assembled solidified linseed oil and method for layer-by-layer self-assembled solidification of compound fat |
| CN106757466A (en) * | 2016-11-28 | 2017-05-31 | 江苏悦达家纺有限公司 | String blending pro-skin fabric and its processing method |
| CN106757494A (en) * | 2016-11-28 | 2017-05-31 | 江苏悦达家纺有限公司 | A kind of pro-skin antibiotic facing material and its processing method |
| CN107042082A (en) * | 2017-06-14 | 2017-08-15 | 温州生物材料与工程研究所 | A kind of aspherical microcapsule granule and preparation method thereof |
| CN108713597A (en) * | 2018-06-01 | 2018-10-30 | 广州富诺营养科技有限公司 | A kind of the health modulation milk beverage and preparation method of addition algae oil DHA |
| CN108936600A (en) * | 2018-05-25 | 2018-12-07 | 姜香 | A method of the rouge ferment that disappears is prepared using brown rice |
| CN109261087A (en) * | 2018-11-28 | 2019-01-25 | 北京尚唐印刷包装有限公司 | Hollow microcapsule and its preparation method and application |
| CN110075156A (en) * | 2019-05-20 | 2019-08-02 | 武汉国粹医药科技有限公司 | A kind of application of elscholtiza micro-capsule and preparation method thereof and elscholtiza micro-capsule |
| WO2020214878A1 (en) * | 2019-04-17 | 2020-10-22 | The Procter & Gamble Company | Methods of making capsules |
| CN112107555A (en) * | 2020-09-18 | 2020-12-22 | 万华化学集团股份有限公司 | Vitamin A acetate microcapsule and preparation method thereof |
| CN112450284A (en) * | 2020-11-27 | 2021-03-09 | 江西恒顶食品有限公司 | Preparation method of linseed oil fat powder |
| CN113209047A (en) * | 2021-03-29 | 2021-08-06 | 上海工程技术大学 | Oxititinib mesylate microcapsule and complex coacervation preparation process thereof |
| CN114176091A (en) * | 2021-12-17 | 2022-03-15 | 扬州工业职业技术学院 | Pesticide microcapsule |
| US11446627B2 (en) | 2019-04-17 | 2022-09-20 | The Procter & Gamble Company | Capsules |
| US11904287B2 (en) | 2019-04-17 | 2024-02-20 | The Procter & Gamble Company | Capsules |
| US11912961B2 (en) | 2020-10-16 | 2024-02-27 | The Procter & Gamble Company | Liquid fabric care compositions comprising capsules |
| US11918441B2 (en) | 2019-04-24 | 2024-03-05 | The Procter & Gamble Company | Highly extensible nonwoven webs and absorbent articles having such webs |
| US11938349B2 (en) | 2020-10-16 | 2024-03-26 | The Procter & Gamble Company | Antiperspirant and deodorant compositions comprising capsules |
| US12077728B2 (en) | 2020-10-16 | 2024-09-03 | The Procter & Gamble Company | Laundry care additive particles |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103142551A (en) * | 2013-04-02 | 2013-06-12 | 黑龙江大学 | Method for preparing micro-capsule by taking xanthan gum and gelatine as wall materials through complex coacervation method |
-
2013
- 2013-08-30 CN CN2013103894463A patent/CN103432970A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103142551A (en) * | 2013-04-02 | 2013-06-12 | 黑龙江大学 | Method for preparing micro-capsule by taking xanthan gum and gelatine as wall materials through complex coacervation method |
Non-Patent Citations (1)
| Title |
|---|
| 蔡明建: "相变蓄能微胶囊性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (26)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103876242B (en) * | 2014-04-01 | 2016-01-20 | 广东工业大学 | Microcapsules of a kind of anti-food-borne pathogens and its production and use |
| CN103876242A (en) * | 2014-04-01 | 2014-06-25 | 广东工业大学 | Microcapsule capable of resisting food-borne pathogenic bacteria as well as preparation method and application thereof |
| CN104496264A (en) * | 2014-12-22 | 2015-04-08 | 江西农业大学 | Method for preparing dry powder organic silicon water repellent microcapsules |
| CN106035739B (en) * | 2016-05-23 | 2019-05-17 | 中国农业大学 | A kind of method that LBL self-assembly solidifies linseed oil and its compounds grease |
| CN106035739A (en) * | 2016-05-23 | 2016-10-26 | 中国农业大学 | Layer-by-layer self-assembled solidified linseed oil and method for layer-by-layer self-assembled solidification of compound fat |
| CN106757466A (en) * | 2016-11-28 | 2017-05-31 | 江苏悦达家纺有限公司 | String blending pro-skin fabric and its processing method |
| WO2018094765A1 (en) * | 2016-11-28 | 2018-05-31 | 江苏悦达家纺有限公司 | Skin-friendly anti-microbial fabric and processing method thereof |
| CN106757494A (en) * | 2016-11-28 | 2017-05-31 | 江苏悦达家纺有限公司 | A kind of pro-skin antibiotic facing material and its processing method |
| CN107042082A (en) * | 2017-06-14 | 2017-08-15 | 温州生物材料与工程研究所 | A kind of aspherical microcapsule granule and preparation method thereof |
| CN108936600A (en) * | 2018-05-25 | 2018-12-07 | 姜香 | A method of the rouge ferment that disappears is prepared using brown rice |
| CN108713597A (en) * | 2018-06-01 | 2018-10-30 | 广州富诺营养科技有限公司 | A kind of the health modulation milk beverage and preparation method of addition algae oil DHA |
| CN109261087A (en) * | 2018-11-28 | 2019-01-25 | 北京尚唐印刷包装有限公司 | Hollow microcapsule and its preparation method and application |
| US11446627B2 (en) | 2019-04-17 | 2022-09-20 | The Procter & Gamble Company | Capsules |
| WO2020214878A1 (en) * | 2019-04-17 | 2020-10-22 | The Procter & Gamble Company | Methods of making capsules |
| US11904287B2 (en) | 2019-04-17 | 2024-02-20 | The Procter & Gamble Company | Capsules |
| US11628413B2 (en) | 2019-04-17 | 2023-04-18 | The Procter & Gamble Company | Methods of making capsules |
| US11918441B2 (en) | 2019-04-24 | 2024-03-05 | The Procter & Gamble Company | Highly extensible nonwoven webs and absorbent articles having such webs |
| CN110075156A (en) * | 2019-05-20 | 2019-08-02 | 武汉国粹医药科技有限公司 | A kind of application of elscholtiza micro-capsule and preparation method thereof and elscholtiza micro-capsule |
| CN110075156B (en) * | 2019-05-20 | 2021-10-15 | 武汉国粹医药科技有限公司 | Elsholtzia ciliata microcapsule, preparation method thereof and application of elsholtzia ciliata microcapsule |
| CN112107555A (en) * | 2020-09-18 | 2020-12-22 | 万华化学集团股份有限公司 | Vitamin A acetate microcapsule and preparation method thereof |
| US11912961B2 (en) | 2020-10-16 | 2024-02-27 | The Procter & Gamble Company | Liquid fabric care compositions comprising capsules |
| US11938349B2 (en) | 2020-10-16 | 2024-03-26 | The Procter & Gamble Company | Antiperspirant and deodorant compositions comprising capsules |
| US12077728B2 (en) | 2020-10-16 | 2024-09-03 | The Procter & Gamble Company | Laundry care additive particles |
| CN112450284A (en) * | 2020-11-27 | 2021-03-09 | 江西恒顶食品有限公司 | Preparation method of linseed oil fat powder |
| CN113209047A (en) * | 2021-03-29 | 2021-08-06 | 上海工程技术大学 | Oxititinib mesylate microcapsule and complex coacervation preparation process thereof |
| CN114176091A (en) * | 2021-12-17 | 2022-03-15 | 扬州工业职业技术学院 | Pesticide microcapsule |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103432970A (en) | Method for preparing organic-inorganic composite microcapsule through complex coacervation | |
| Reis et al. | Review and current status of emulsion/dispersion technology using an internal gelation process for the design of alginate particles | |
| Liu et al. | Preparation of monodisperse calcium alginate microcapsules via internal gelation in microfluidic-generated double emulsions | |
| Zhao et al. | Hybrid nanostructured particles via surfactant-free double miniemulsion polymerization | |
| US9068109B2 (en) | Nano-encapsulated triggered-release viscosity breaker | |
| Tissot et al. | Hybrid latex particles coated with silica | |
| Shi et al. | Release behavior of thin-walled microcapsules composed of polyelectrolyte multilayers | |
| Szczepanowicz et al. | Encapsulation of liquid cores by layer-by-layer adsorption of polyelectrolytes | |
| CN104128136B (en) | Micro-nano gel particles and its controllable method for preparing and application | |
| Szczepanowicz et al. | Formation of oil filled nanocapsules with silica shells modified by sequential adsorption of polyelectrolytes | |
| CN102167885A (en) | High-intensity urea-formaldehyde resin microcapsule and preparation method thereof | |
| Naseem et al. | Platinum nanoparticles fabricated multiresponsive microgel composites: synthesis, characterization, and applications | |
| IL269819B (en) | Additive manufacturing support material | |
| CN103127031A (en) | Preparation method for oily and oil soluble drug nanocapsules | |
| JP2014087786A (en) | Method for manufacturing microcapsule and microcapsule | |
| da Silva et al. | Stöber method and its nuances over the years | |
| Liu et al. | Three-fluid nozzle spray drying strategy for efficient fabrication of functional colloidosomes | |
| DE102010003615A1 (en) | Process for the preparation of a drug delivery system based on polyelectrolyte complexes | |
| Goller et al. | Silica encapsulation of liquid PDMS droplets | |
| CN101386671B (en) | Method for preparing environmental responsibility mesoporous silicon sphere | |
| CN109276560B (en) | Lactoferrin-containing pH response type microcapsule and preparation method and application thereof | |
| CN108355591A (en) | Dimethyl silicone polymer causes ethyl cellulose phase separation and prepares microcapsule method | |
| Ullrich et al. | Formation of multi-compartmental particles by controlled aggregation of liposomes | |
| CN104829793A (en) | Preparation method of temperature and pH sensitive organic/inorganic hybrid material POSS/PDMAEMA-b-PNIPAM | |
| CN103768038B (en) | Fibroin albumen one pack system microcapsule, fibroin albumen-nanometer gold hybridized microcapsule and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20131211 |