CN1586709A - Process for preparing polyhydroxy acid ester micro capsule - Google Patents
Process for preparing polyhydroxy acid ester micro capsule Download PDFInfo
- Publication number
- CN1586709A CN1586709A CN 200410068846 CN200410068846A CN1586709A CN 1586709 A CN1586709 A CN 1586709A CN 200410068846 CN200410068846 CN 200410068846 CN 200410068846 A CN200410068846 A CN 200410068846A CN 1586709 A CN1586709 A CN 1586709A
- Authority
- CN
- China
- Prior art keywords
- acid ester
- polyhydroxy acid
- solvent
- capsule
- micro
- 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.)
- Granted
Links
- 239000003094 microcapsule Substances 0.000 title claims abstract description 44
- 229920001273 Polyhydroxy acid Polymers 0.000 title claims abstract description 41
- 150000002148 esters Chemical class 0.000 title claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 title description 3
- 239000000463 material Substances 0.000 claims abstract description 33
- 239000002904 solvent Substances 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 229920000642 polymer Polymers 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 239000003381 stabilizer Substances 0.000 claims abstract description 5
- 239000004094 surface-active agent Substances 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 9
- 230000002045 lasting effect Effects 0.000 claims description 2
- 239000000725 suspension Substances 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 9
- -1 hydroxy acid ester Chemical class 0.000 abstract description 5
- 229920001577 copolymer Polymers 0.000 abstract 1
- 239000003607 modifier Substances 0.000 abstract 1
- 239000002861 polymer material Substances 0.000 abstract 1
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 24
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 15
- 239000002775 capsule Substances 0.000 description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 7
- 239000000843 powder Substances 0.000 description 5
- 229920002367 Polyisobutene Polymers 0.000 description 4
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 4
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 description 3
- 235000019743 Choline chloride Nutrition 0.000 description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 3
- GHASVSINZRGABV-UHFFFAOYSA-N Fluorouracil Chemical compound FC1=CNC(=O)NC1=O GHASVSINZRGABV-UHFFFAOYSA-N 0.000 description 3
- 229960003178 choline chloride Drugs 0.000 description 3
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 235000003891 ferrous sulphate Nutrition 0.000 description 3
- 239000011790 ferrous sulphate Substances 0.000 description 3
- 229960002949 fluorouracil Drugs 0.000 description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002778 food additive Substances 0.000 description 2
- 235000013373 food additive Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 230000000035 biogenic effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
Landscapes
- Manufacturing Of Micro-Capsules (AREA)
- Medicinal Preparation (AREA)
Abstract
The preparation process of polyhydroxy acid ester microcapsule features the microcapsule material of hydroxy acid ester polymer, copolymer or mixture and includes the following steps: adding the matter to be encapsulated into hydroxy acid ester polymer solution of 2-20 % concentration to form suspension; adding non-solvent, which does not dissolve the encapsulated matter and hydroxy acid ester polymer, in the 2-5 times volume of solvent for completely dissolving the hydroxy acid ester polymer material under the room temperature and stirring condition to form microcapsule; adding non-solvent in the same volume to solidify microcapsule; and adding optional supplementary material, such as surfactant, anti-sticking agent, modifier and stabilizer. The present invention has the features of simple technological process, easy control, high yield and high encapsulating rate.
Description
Technical field
The preparation method of polyhydroxy acid ester micro capsule belongs to the micro-capsule preparing technical field, and it is to utilize the solvent-nonsolvent legal system to be equipped with a kind of method of polyhydroxy acid ester micro capsule in definite saying.
Background technology
At the initial stage fifties, the pigment capsule is used for the production of carbonless copy paper.Since then, the microcapsules development rapidly.Its typical application has coating, composite, extinguish material, various daily chemicals, adhesive, medical material etc.Biogenic polyhydroxy acid ester be a class have biocompatibility, optical activity, thermoplasticity and can be in vivo with natural environment in the boiomacromolecule of degraded fully, have great application prospect as bioactive materials and degradation plastic at chemical field.At present, both at home and abroad be with the polyhydroxy acid ester material microencapsulation research seldom, only 18 pieces of pertinent literatures, related manufacturing processes only have complex process, intra-liquid desiccation method that envelop rate is lower (to comprise emulsification, emulsion-liquid drying method; Solvent evaporated method) and the report of the demanding supercritical extraction of equipment intra-liquid desiccation method is called again:, limited broad research and the application in this respect of this technology.
Summary of the invention
The objective of the invention is: adopt a kind of technology simple, easily and control, productive rate height, new method that envelop rate is high prepare polyhydroxy acid ester micro capsule, this method can be used for the microencapsulation in fields such as medicine, cosmetics, food additives, feed addictive, agricultural chemicals.
The invention is characterized in that it contains following steps successively:
(1) encapsulated material is suspended in the solution of the polyhydroxy acid ester material that adds required auxiliary material:
Described polyhydroxy acid ester as the microencapsulation material is any in the blend of polyhydroxy acid esters polymer, polyhydroxy acid lipin polymer, polyhydroxy acid ester and other materials, and polyhydroxy acid ester material solution concentration is 2~20%;
The solvent of described preparation polyhydroxy acid ester material solution is the solvent that can dissolve polyhydroxy acid ester fully;
Described required auxiliary material is meant surfactant or antiplastering aid or dressing agent and stabilizing agent;
(2) under room temperature and lasting stirring condition, have to suspendible that to add volume ratio in the polyhydroxy acid ester solution of encapsulated material be the non-solvent of 2~5 times of the described solvent volume of step (1), described non-solvent is not for dissolving the solvent of encapsulated material and polyhydroxy acid ester, to generate micro-capsule, in non-solvent, can add auxiliary material, as antiplastering aid or dressing agent and stabilizing agent;
(3) treat that micro-capsule generates after, add again and the identical non-solvent of the described volume ratio of step (2), with curing microcapsules;
(4) drying under reduced pressure under the room temperature, sieve and collect micro-capsule.
Advantage of the present invention is: use the microencapsulation that this method can be used for multiple material, and technology is simple, easily and control, productive rate height (>90%), envelop rate height (>90%), can produce by batch in a large number.
The specific embodiment:
Below in conjunction with embodiment the present invention is further illustrated, but not only be confined to listed embodiment.
Embodiment 1:
Field of medicaments
(a) fluorouracil micro-capsule
Composition
Fluorouracil 1.0g
Polyhydroxy acid ester 3.0g
Polyisobutene 0.15g
Chloroform 30ml
Cyclohexane 180ml
Polyhydroxy acid ester (capsule material) is dissolved in the chloroform, adds the fluorouracil medicine powder, make to form stable suspension; Polyisobutene is dissolved in the 90ml cyclohexane, continue stirs down, slowly splash in material-encapsulated thing suspension number, treat to add 90ml cyclohexane curing microcapsules 30min again after micro-capsule generates, drying under reduced pressure sieves and collects micro-capsule under the room temperature.
(b) magnetic micro-capsule
Composition
Fe
3O
4 0.5g
Polyhydroxy acid ester 2.0g
Polyisobutene 0.16g
Chloroform 20ml
Benzinum 120ml
Polyhydroxy acid ester (capsule material) is dissolved in the chloroform, adds Fe
3O
4Powder makes to form stable suspension; Polyisobutene is dissolved in the 60ml benzinum, continue stirs down, slowly splash in material-encapsulated thing suspension number, treat to add 60ml benzinum curing microcapsules 30min again after micro-capsule generates, drying under reduced pressure sieves and collects micro-capsule under the room temperature.
Embodiment 2:
The food additives field
(a) citric acid micro-capsule
Composition
Citric acid 0.5g
Polyhydroxy acid ester 2.0g
Span?80 0.12g
Chloroform 20ml
Benzinum 120ml
Polyhydroxy acid ester (capsule material), Span 80 are dissolved in the chloroform, add the citric acid powder, make to form stable suspension; Continue to stir down, slowly drip the 60ml benzinum to material-encapsulated thing suspension number, treat to add 60ml benzinum curing microcapsules 30min again after micro-capsule generates, drying under reduced pressure sieves and collects micro-capsule under the room temperature.
(b) monascorubin micro-capsule
Monascorubin 0.5g
Polyhydroxy acid ester 2.0g
Span?80 0.12g
Chloroform 20ml
Benzinum 120ml
Polyhydroxy acid ester (capsule material), Span 80 are dissolved in the chloroform, add the monascorubin powder, make to form stable suspension; Continue to stir down, slowly drip the 60ml benzinum to material-encapsulated thing suspension number, treat to add 60ml benzinum curing microcapsules 30min again after micro-capsule generates, drying under reduced pressure sieves and collects micro-capsule under the room temperature.
(c) ferrous sulfate micro-capsule
Ferrous sulfate 0.5g
Polyhydroxy acid ester 2.0g
Span?80 0.12g
Chloroform 20ml
Benzinum 120ml
Polyhydroxy acid ester (capsule material), Span 80 are dissolved in the chloroform, add the ferrous sulfate powder, make to form stable suspension; Continue to stir down, slowly drip the 60ml benzinum to material-encapsulated thing suspension number, treat to add 60ml benzinum curing microcapsules 30min again after micro-capsule generates, drying under reduced pressure sieves and collects micro-capsule under the room temperature.
Embodiment 3:
Feed additive field
The Choline Chloride micro-capsule
Composition
Choline Chloride 0.5g
Polyhydroxy acid ester 2.0g
Span?80 0.12g
Chloroform 20ml
Benzinum 120ml
Polyhydroxy acid ester (capsule material), Span 80 are dissolved in the chloroform, add the Choline Chloride powder, make to form stable suspension; Continue to stir down, slowly drip the 60ml benzinum to material-encapsulated thing suspension number, treat to add 60ml benzinum curing microcapsules 30min again after micro-capsule generates, drying under reduced pressure sieves and collects micro-capsule under the room temperature.
Claims (1)
1. the preparation method of polyhydroxy acid ester micro capsule is characterized in that, it contains following steps successively:
(1) encapsulated material is suspended in the solution of the polyhydroxy acid ester material that adds required auxiliary material:
Described polyhydroxy acid ester as the microencapsulation material is any in the blend of polyhydroxy acid esters polymer, polyhydroxy acid lipin polymer, polyhydroxy acid ester and other materials, and polyhydroxy acid ester material solution concentration is 2~20%;
The solvent of described preparation polyhydroxy acid ester material solution is the solvent that can dissolve polyhydroxy acid ester fully;
Described required auxiliary material is meant surfactant or antiplastering aid or dressing agent and stabilizing agent;
(2) under room temperature and lasting stirring condition, have to suspendible that to add volume ratio in the polyhydroxy acid ester solution of encapsulated material be the non-solvent of 2~5 times of the described solvent volume of step (1), described non-solvent is not for dissolving the solvent of encapsulated material and polyhydroxy acid ester, to generate micro-capsule, in non-solvent, can add auxiliary material, as antiplastering aid or dressing agent and stabilizing agent;
(3) treat that micro-capsule generates after, add again and the identical non-solvent of the described volume ratio of step (2), with curing microcapsules;
(4) drying under reduced pressure under the room temperature, sieve and collect micro-capsule.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2004100688465A CN100411726C (en) | 2004-07-09 | 2004-07-09 | Process for preparing polyhydroxy acid ester micro capsule |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2004100688465A CN100411726C (en) | 2004-07-09 | 2004-07-09 | Process for preparing polyhydroxy acid ester micro capsule |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1586709A true CN1586709A (en) | 2005-03-02 |
CN100411726C CN100411726C (en) | 2008-08-20 |
Family
ID=34604178
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNB2004100688465A Expired - Fee Related CN100411726C (en) | 2004-07-09 | 2004-07-09 | Process for preparing polyhydroxy acid ester micro capsule |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN100411726C (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107753463A (en) * | 2017-11-23 | 2018-03-06 | 铜陵市宏达家电有限责任公司 | Sulfadimidine micro-capsule and preparation method thereof |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP3199818B2 (en) * | 1992-03-06 | 2001-08-20 | 松本油脂製薬株式会社 | Microcapsules for epoxy resin curing agent |
CN1155394C (en) * | 2002-07-25 | 2004-06-30 | 无锡健特药业有限公司 | Microcapsule coated trace element product and its producing method |
-
2004
- 2004-07-09 CN CNB2004100688465A patent/CN100411726C/en not_active Expired - Fee Related
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107753463A (en) * | 2017-11-23 | 2018-03-06 | 铜陵市宏达家电有限责任公司 | Sulfadimidine micro-capsule and preparation method thereof |
Also Published As
Publication number | Publication date |
---|---|
CN100411726C (en) | 2008-08-20 |
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C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
C17 | Cessation of patent right | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080820 Termination date: 20120709 |