CN103769017B - A kind of Microencapsulation Method of water-soluble inorganic salt - Google Patents
A kind of Microencapsulation Method of water-soluble inorganic salt Download PDFInfo
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- CN103769017B CN103769017B CN201210405628.0A CN201210405628A CN103769017B CN 103769017 B CN103769017 B CN 103769017B CN 201210405628 A CN201210405628 A CN 201210405628A CN 103769017 B CN103769017 B CN 103769017B
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Abstract
The invention discloses a kind of Microencapsulation Method of water-soluble inorganic salt; By adding macromolecule wall material in organic solvent, being stirred to wall material and dissolving completely, form oil phase A
0; At oil phase A
0in add surfactant and cosurfactant, form oil-phase solution A; Add water-soluble inorganic salt in deionized water, form aqueous phase solution B; Solution B is slowly joined in solution A, stirs, form w/o type emulsion; In w/o type emulsion, add protectiveness liquid, add non-solvent afterwards, macromolecule wall material is separated out, and deposits to water-soluble inorganic salt surface, obtains the microcapsules of water-soluble inorganic salt; The method is more economical, practical, efficient, and the Microcapsules Size of preparation is little, good dispersion.
Description
Technical field
The present invention relates to the microencapsulation of inorganic salts, particularly relate to a kind of Microencapsulation Method of water-soluble inorganic salt.
Background technology
Microcapsules technology utilizes natural or synthesized polymer material as shell material, using coated as core material to solid, liquid or gas, forms the technology of a kind of microencapsulation with semi permeability or sealing cyst membrane.The diameter of microcapsules is generally 1 μm ~ 1mm.Although the preparation method of microcapsules is numerous, diverse ways has the core and wall material that adapt with it.
Water-soluble inorganic salt has a wide range of applications in chemicals synthesis with production as phase-change material, reversible temperature indicating material, food or medicated premix.Therefore, the microencapsulation realizing water-soluble inorganic salt is extremely important.Water-soluble material micro-encapsulation technology is complicated, and the document of current water-soluble inorganic salt microcapsule preparation method is relatively less, mainly spray drying process, spray condensation method and oil-phase separating method.Simply, easy to operate, sustained release performance is good for spray condensation method and spray drying process preparation technology, but obtained microcapsule product compactness is poor, and particle diameter is relatively large.Microcapsules prepared by oil-phase separating method easily produce adhesion, gathering, and particle diameter is larger, and domain size distribution is wider; For needing small particle diameter, there is certain restriction in the microcapsule product of narrow diameter distribution.
Liu too very waits (Liu Taiqi; Grasp refined; Zhang Cheng; Chen Xi; Yu Jianxiang. the research of " New Technologies " heat processing technique technique and material .2010,3,81-85) adopt solvent evaporated method, be wall material with polymethyl methacrylate, to CaCl
26H
2it is 79.12 μm of microencapsulated phase change materials that O carries out coated particle diameter of having prepared.(the Xu Jianming such as Xu Jianming; Liu Zuliang; Zhai Dandan. Liaoning chemical industry .2003,32,142-143) utilize physical and chemical principle to be separated, carry out coated to the saturated solution of ammonium nitrate, obtain the microcapsules of domain size distribution between 20 ~ 344.37 μm.Superfine (the Qiao Jichao of Qiao Ji; Hu little Ling; Guan Ping. Micrometer-Nanometer Processing Technology .2007,3,43-47) with ethyl cellulose and polyethylene for shell material, thermosensitive chromotropic material cobalt chloride is core material, adopt oil-phase separating method, macromolecular material carried out to thermosensitive chromotropic material cobalt chloride coated, prepared size homogeneous, be uniformly dispersed, diameter is about the reversible temperature indicating microcapsules of 4.5 μm.The Microcapsules Size of preparation is little, and domain size distribution is narrow, but preparation technology's more complicated, and manufacturing cycle is long, thus makes preparation cost higher.
Summary of the invention
The technical problem that will solve of the present invention is the shortcoming overcoming prior art, a kind of more economical, practical, method of preparing small particle diameter, the dispersed microencapsulation of water-soluble inorganic salt preferably is efficiently provided, and microencapsulation technology is extended to application that is darker, that upgrade.
The invention provides a kind of Microencapsulation Method of water-soluble inorganic salt, comprise the following steps:
1) prepare raw material, prepare each raw material according to following parts by weight:
Organic solvent 10 ~ 75 parts;
Macromolecule wall material 0.3 ~ 4.0 part;
Surfactant sorbitol anhydride oleate 0.5 ~ 5 part;
Cosurfactant aluminum stearate 0.3 ~ 3 part;
Deionized water 1 ~ 10 part;
Water-soluble inorganic salt 0.5 ~ 8 part;
Atoleine 5 ~ 90 parts;
Non-solvent 3 ~ 60 parts;
2) add macromolecule wall material in organic solvent, be stirred to wall material and dissolve completely, form oil phase A
0; At oil phase A
0in add surfactant and cosurfactant, form oil-phase solution A;
3) add water-soluble inorganic salt in deionized water, form aqueous phase solution B;
4) solution B is slowly joined in solution A, stir, form w/o type emulsion; In w/o type emulsion, add protectiveness liquid, add non-solvent afterwards, macromolecule wall material is separated out, and deposits to water-soluble inorganic salt surface, obtains the microcapsules of water-soluble inorganic salt;
When described macromolecule wall material is ethyl cellulose: described organic solvent is carrene, described non-solvent is n-hexane; Described organic solvent is chloroform, and described non-solvent is benzinum; Described organic solvent is toluene, and described non-solvent is benzinum; Described organic solvent is ethyl acetate, and described non-solvent is n-hexane;
When described macromolecule wall material is carboxymethylethylcellulose: described organic solvent is methyl acetate, described non-solvent is ether;
When described macromolecule wall material is polyethylene: described organic solvent is dimethylbenzene, described non-solvent is ethanol;
When described macromolecule wall material is polyvinyl acetate: described organic solvent is chloroform, described non-solvent is ethanol.
Take out the microcapsules sample of the water-soluble inorganic salt obtained, first wash 3 times with non-solvent, then spend deionized water 3 times, dry, obtain final microcapsule product.
In reaction system, the solution of water-soluble inorganic salt is all neutral, and whole reaction does not need to consider pH value.
Described water-soluble inorganic salt is inorganic alkaline metal salt.As: potassium chloride, calcium chloride, calcium nitrate etc.
Described atoleine is protectiveness liquid.
Described step 4) stir speed (S.S.) is 250 ~ 1200r/min.
Above-mentioned reaction is carried out at normal temperatures.
Compared with prior art, the invention has the beneficial effects as follows:
1, this method preparation technology is simple, and manufacturing cycle is short, and whole course of reaction is all carry out at normal temperatures, and cost is reduced further.
2, this method is on the basis using surfactant, adds cosurfactant again, and make the w/o type emulsion of formation more stable, the Microcapsules Size of formation is less.
3, the microcapsules that prepared by prior art oil-phase separating method easily produce the defect such as adhesion, gathering, and this method adds protectiveness solution and atoleine, and the dispersiveness of the microcapsules obtained is improved.
Accompanying drawing explanation
Fig. 1 is the microcapsules multiplication factor of water-soluble inorganic salt prepared by the present invention is the scanning electron microscope diagram of 1.5K.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the invention will be further described.
Embodiment 1
In 20g carrene, add 1.0g ethyl cellulose, be stirred to ethyl cellulose and dissolve completely, form oil phase A
0; To above-mentioned oil phase A
0in add 2g surface light activating agent span80(sorbitol anhydride oleate) and 0.7g cosurfactant aluminum stearate form oil-phase solution A; In 5.0g deionized water, add 1.2g water-soluble inorganic salt potassium chloride, form aqueous phase solution B; Solution B is slowly joined in solution A, under 600r/min stir speed (S.S.), forms stable w/o type emulsion; In above-mentioned emulsion, add 18g atoleine and 6.5g non-solvent n-hexane, isolate microcapsules; Respectively with n-hexane and deionized water washing, suction filtration, drying, obtain the microcapsules of potassium chloride.
Embodiment 2
In 15g chloroform, add 0.5g ethyl cellulose, be stirred to ethyl cellulose and dissolve completely, form oil phase A
0; To above-mentioned oil phase A
0in add 1.0g surface light activating agent span80 and 0.3g cosurfactant aluminum stearate and form oil-phase solution A; In 3.0g deionized water, add 1.5g water-soluble inorganic salt calcium chloride, form aqueous phase solution B; Solution B is slowly joined in solution A, under 400r/min stir speed (S.S.), forms stable w/o type emulsion; In above-mentioned emulsion, add 18g atoleine and 13g non-solvent benzinum, isolate microcapsules; Respectively with benzinum and deionized water washing, suction filtration, drying, obtain the microcapsules of calcium chloride.
Embodiment 3
In 11g toluene, add 0.6g ethyl cellulose, be stirred to ethyl cellulose and dissolve completely, form oil phase A
0; To above-mentioned oil phase A
0in add 1.4g surface light activating agent span80 and 0.6g cosurfactant aluminum stearate and form oil-phase solution A; In 3.0g deionized water, add 1.5g water-soluble inorganic salt calcium chloride, form aqueous phase solution B; Solution B is slowly joined in solution A, under 800r/min stir speed (S.S.), forms stable w/o type emulsion; In above-mentioned emulsion, add 18g atoleine and 10g non-solvent benzinum, isolate microcapsules; Respectively with benzinum and deionized water washing, suction filtration, drying, obtain the microcapsules of calcium chloride.
Embodiment 4
In 13g dimethylbenzene, add 1.2g polyethylene, be stirred to polyethylene and dissolve completely, form oil phase A
0; To above-mentioned oil phase A
0in add 1.8g surface light activating agent span80 and 1.0g cosurfactant aluminum stearate and form oil-phase solution A; In 4.0g deionized water, add 4.5g water-soluble inorganic salt calcium nitrate, form aqueous phase solution B; Solution B is slowly joined in solution A, under 1000r/min stir speed (S.S.), forms stable w/o type emulsion; In above-mentioned emulsion, add 18g atoleine and 24g non-solvent ethanol, isolate microcapsules; Respectively with ethanol and deionized water washing, suction filtration, drying, obtain the microcapsules of calcium nitrate.
Embodiment 5
In 18g ethyl acetate, add 1.8g ethyl cellulose, be stirred to ethyl cellulose and dissolve completely, form oil phase A
0; To above-mentioned oil phase A
0in add 2.0g surface light activating agent span80 and 1.2g cosurfactant aluminum stearate and form oil-phase solution A; In 8.0g deionized water, add 5.0g water-soluble inorganic salt calcium chloride, form aqueous phase solution B; Solution B is slowly joined in solution A, under 1000r/min stir speed (S.S.), forms stable w/o type emulsion; In above-mentioned emulsion, add 18g atoleine and 24g non-solvent n-hexane, isolate microcapsules; Respectively with n-hexane and deionized water washing, suction filtration, drying, obtain the microcapsules of calcium chloride.
Embodiment 6
In 10g methyl acetate, add 0.6g carboxymethylethylcellulose, be stirred to carboxymethylethylcellulose and dissolve completely, form oil phase A
0; To above-mentioned oil phase A
0in add 1.2g surface light activating agent span80 and 0.8g cosurfactant aluminum stearate and form oil-phase solution A; In 3.0g deionized water, add 1.0g water-soluble inorganic salt calcium chloride, form aqueous phase solution B; Solution B is slowly joined in solution A, under 400r/min stir speed (S.S.), forms stable w/o type emulsion; In above-mentioned emulsion, add 13g atoleine and 20g non-solvent ether, isolate microcapsules; Respectively with ether and deionized water washing, suction filtration, drying, obtain the microcapsules of calcium chloride.
Embodiment 7
In 15g chloroform, add 0.5g polyvinyl acetate, be stirred to polyvinyl acetate and dissolve completely, form oil phase A
0; To above-mentioned oil phase A
0in add 1.0g surface light activating agent span80 and 0.3g cosurfactant aluminum stearate and form oil-phase solution A; In 3.0g deionized water, add 1.5g water-soluble inorganic salt calcium chloride, form aqueous phase solution B; Solution B is slowly joined in solution A, under 400r/min stir speed (S.S.), forms stable w/o type emulsion; In above-mentioned emulsion, add 18g atoleine and 13g non-solvent ethanol, isolate microcapsules; Respectively with ethanol and deionized water washing, suction filtration, drying, obtain the microcapsules of calcium chloride.
Comparative example
With embodiment 1, difference is, does not add cosurfactant aluminum stearate and liquid petroleum.
Microcapsules Size is compared with embodiment, obviously comparatively large, and disperses bad.
Obviously; the above embodiment of the present invention is only for example of the present invention is clearly described; and be not the restriction to embodiments of the present invention; for those of ordinary skill in the field; can also make other changes in different forms on the basis of the above description; here cannot give exhaustive to all embodiments, every belong to technical scheme of the present invention the apparent change of extending out or variation be still in the row of protection scope of the present invention.
Claims (1)
1. a Microencapsulation Method for water-soluble inorganic salt, is characterized in that, comprises the following steps:
1) prepare raw material, prepare each raw material according to following parts by weight:
Organic solvent 10 ~ 75 parts;
Macromolecule wall material 0.3 ~ 4.0 part;
Surfactant sorbitol anhydride oleate 0.5 ~ 5 part;
Cosurfactant aluminum stearate 0.3 ~ 3 part;
Deionized water 1 ~ 10 part;
Water-soluble inorganic salt 0.5 ~ 8 part;
Atoleine 5 ~ 90 parts;
Non-solvent 3 ~ 60 parts;
2) add macromolecule wall material in organic solvent, be stirred to wall material and dissolve completely, form oil phase A
0; At oil phase A
0in add surfactant and cosurfactant, form oil-phase solution A;
3) add water-soluble inorganic salt in deionized water, form aqueous phase solution B;
4) solution B is slowly joined in solution A, stir, form w/o type emulsion; In w/o type emulsion, add atoleine, add non-solvent afterwards, macromolecule wall material is separated out, and deposits to water-soluble inorganic salt surface, obtains the microcapsules of water-soluble inorganic salt;
When described macromolecule wall material is ethyl cellulose: when described organic solvent is carrene, described non-solvent is n-hexane;
When described macromolecule wall material is ethyl cellulose: when described organic solvent is chloroform, described non-solvent is benzinum;
When described macromolecule wall material is ethyl cellulose: when described organic solvent is toluene, described non-solvent is benzinum;
When described macromolecule wall material is ethyl cellulose: when described organic solvent is ethyl acetate, described non-solvent is n-hexane;
When described macromolecule wall material is carboxymethylethylcellulose: described organic solvent is methyl acetate, described non-solvent is ether;
When described macromolecule wall material is polyethylene: described organic solvent is dimethylbenzene, described non-solvent is ethanol;
When described macromolecule wall material is polyvinyl acetate: described organic solvent is chloroform, described non-solvent is ethanol.
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| CN104069087B (en) * | 2014-07-15 | 2017-03-08 | 中国科学院理化技术研究所 | A kind of microcapsule for the treatment of microwave tumor enhanced sensitivity and its preparation method and application |
| CN105032313B (en) * | 2015-07-23 | 2017-04-26 | 北京宇田相变储能科技有限公司 | Water soluble salt microcapsule wrapped by polybenzoxazine resin and preparation method thereof |
| CN109261090A (en) * | 2018-10-08 | 2019-01-25 | 长春理工大学 | A kind of preparation method of phase-change microcapsule |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1844269A (en) * | 2006-05-08 | 2006-10-11 | 清华大学深圳研究生院 | Phase-transition energy-storage microcapsules and their preparing process |
| CN100522145C (en) * | 2006-12-14 | 2009-08-05 | 东南大学 | Preparation process of nano drug-loaded biological micro-capsule |
| CN101564667A (en) * | 2009-05-19 | 2009-10-28 | 无锡福尔顺科技有限公司 | Method for preparing alginate soft capsule |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1844269A (en) * | 2006-05-08 | 2006-10-11 | 清华大学深圳研究生院 | Phase-transition energy-storage microcapsules and their preparing process |
| CN100522145C (en) * | 2006-12-14 | 2009-08-05 | 东南大学 | Preparation process of nano drug-loaded biological micro-capsule |
| CN101564667A (en) * | 2009-05-19 | 2009-10-28 | 无锡福尔顺科技有限公司 | Method for preparing alginate soft capsule |
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