CN100411726C - Process for preparing polyhydroxy acid ester micro capsule - Google Patents

Process for preparing polyhydroxy acid ester micro capsule Download PDF

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Publication number
CN100411726C
CN100411726C CNB2004100688465A CN200410068846A CN100411726C CN 100411726 C CN100411726 C CN 100411726C CN B2004100688465 A CNB2004100688465 A CN B2004100688465A CN 200410068846 A CN200410068846 A CN 200410068846A CN 100411726 C CN100411726 C CN 100411726C
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China
Prior art keywords
acid ester
polyhydroxy acid
capsule
solvent
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.)
Expired - Fee Related
Application number
CNB2004100688465A
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Chinese (zh)
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CN1586709A (en
Inventor
谭丰苹
丁富新
蒋国强
昝佳
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Tsinghua University
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Tsinghua University
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Priority to CNB2004100688465A priority Critical patent/CN100411726C/en
Publication of CN1586709A publication Critical patent/CN1586709A/en
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Publication of CN100411726C publication Critical patent/CN100411726C/en
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  • Manufacturing Of Micro-Capsules (AREA)
  • Medicinal Preparation (AREA)

Abstract

The present invention relates to a method for preparing a polyhydroxy acid ester microcapsule, which belongs to the technical field of the preparation of microcapsules. The present invention is characterized in that a polymer of polyhydroxy acid ester or a copolymer or a blending object is used as microcapsulization materials, and materials to be sealed are added to a polyhydroxy acid ester solution with the concentration of 2 to 20% to form a suspension solution. A nonsolvent for completely dissolving polyhydroxy acid ester solution is added to the suspension solution at a room temperature and under the condition of stirring continuously, wherein the volume of the nonsolvent is two to five times of that of the polyhydroxy acid ester solution. After microcapsules are generated, nonsolvent solidified microcapsules with the same volume are added to the suspension solution. The nonsolvent is a solvent which is insoluble in sealed substances and the polyhydroxy acid ester. Auxiliary materials can be added to the polyhydroxy acid ester solution or the nonsolvent, and the auxiliary materials comprise surface active agents or antisticking agents or modifying agents or stabilizing agents. The present invention has the characteristics of simple technology, easy control, high yield and high encapsulation efficiency.

Description

A kind of preparation method of polyhydroxy acid ester micro capsule
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 ester polymer, polyhydroxy acid ester copolymer, polyhydroxy acid ester and other materials, and polyhydroxy acid ester material solution concentration is 2~20%;
The solvent for preparing described 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 or stabilizing agent;
(2) under room temperature and lasting stirring condition, to suspendible have add in the polyhydroxy acid ester solution of encapsulated material volume ratio be 2~5 times of the described solvent volume of step (1) to encapsulated material and the undissolved solvent of polyhydroxy acid ester, to generate micro-capsule, in this solvent, add antiplastering aid or dressing agent or stabilizing agent;
(3) treat that micro-capsule generates after, it is described to encapsulated material and the undissolved solvent of polyhydroxy acid ester, with curing microcapsules to add the step (2) identical with the described volume ratio of step (2) again;
(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 ester polymer, polyhydroxy acid ester copolymer, polyhydroxy acid ester and other materials, and polyhydroxy acid ester material solution concentration is 2~20%;
The solvent for preparing described 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 or stabilizing agent;
(2) under room temperature and lasting stirring condition, to suspendible have add in the polyhydroxy acid ester solution of encapsulated material volume ratio be 2~5 times of the described solvent volume of step (1) to encapsulated material and the undissolved solvent of polyhydroxy acid ester, to generate micro-capsule, in this solvent, add antiplastering aid or dressing agent or stabilizing agent;
(3) treat that micro-capsule generates after, it is described to encapsulated material and the undissolved solvent of polyhydroxy acid ester, with curing microcapsules to add the step (2) identical with the described volume ratio of step (2) again;
(4) drying under reduced pressure under the room temperature, sieve and collect micro-capsule.
CNB2004100688465A 2004-07-09 2004-07-09 Process for preparing polyhydroxy acid ester micro capsule Expired - Fee Related CN100411726C (en)

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

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CN1586709A CN1586709A (en) 2005-03-02
CN100411726C true CN100411726C (en) 2008-08-20

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Families Citing this family (1)

* Cited by examiner, † Cited by third party
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

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05247179A (en) * 1992-03-06 1993-09-24 Matsumoto Yushi Seiyaku Co Ltd Microcapsule for epoxy resin curing agent
CN1391903A (en) * 2002-07-25 2003-01-22 无锡健特药业有限公司 Microcapsule coated trace element product and its producing method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05247179A (en) * 1992-03-06 1993-09-24 Matsumoto Yushi Seiyaku Co Ltd Microcapsule for epoxy resin curing agent
CN1391903A (en) * 2002-07-25 2003-01-22 无锡健特药业有限公司 Microcapsule coated trace element product and its producing method

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Granted publication date: 20080820

Termination date: 20120709