CN101513394B - Continuous preparation method for nanometer dispersed vitamin A microcapsule - Google Patents
Continuous preparation method for nanometer dispersed vitamin A microcapsule Download PDFInfo
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- CN101513394B CN101513394B CN2009100970647A CN200910097064A CN101513394B CN 101513394 B CN101513394 B CN 101513394B CN 2009100970647 A CN2009100970647 A CN 2009100970647A CN 200910097064 A CN200910097064 A CN 200910097064A CN 101513394 B CN101513394 B CN 101513394B
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Abstract
The invention discloses a continuous preparation method for nanometer dispersed vitamin A microcapsule, comprising the following steps: the vitamin A crystal, the antioxidant and the solvent are ground until the particle size of the vitamin A is 2 to 5 mu m, the vitamin A dispersion liquid is prepared; the vitamin A dispersion liquid is heated by a preheater and dissolved and cooled, then the solution is sent into a crystallizer of the supergravity rotating packed bed with the liquid distributor, at the same time the water solution with protection colloid is sent into the above crystallizer of the supergravity rotating packed bed, the nanometer dispersed vitamin A dispersion liquid is obtained at the outlet, the dispersion liquid is in spray drying in the spray drying device with fluidization cooling device to obtain the nanometer dispersed vitamin A microcapsule. The invention has the advantage of continuous production, because the vitamin A crystal grain in the product is small, the product has wide application and high bioavailability.
Description
Technical field
The present invention relates to a kind of preparation method of serialization nanometer dispersed vitamin A microcapsule, be specifically related to adopt the hypergravity RPB to carry out the preparation of serialization nanometer dispersed vitamin A microcapsule.
Background technology
It is one of the world's four big nutrient deficiency diseases that vitamin A (VA) lacks, and always pays close attention to for researcher.VA is admitted to the important function of body vision, growth promoter and reproduction.In recent years, more domestic researchs find that also VA lacks or can not influence completely other function of body, mainly contains: immunologic function; Hemopoietic and cell receptor function; Iron metabolism; VA lacks also can cause respiratory tract, intestinal mucosa epithelium keratinization, increases the susceptibility of body to respiratory tract, intestinal infection disease; Influence burn, wound and wound healing after operation; Can make under wet heat condition in the blood that SOD is active to descend, MDA concentration raises, and lipid peroxidation injury increases the weight of etc.In animal husbandry, the function of VA is also most important.VA lacks and easily causes animal miscarriage, difficult labour; The reproduction of male animal ability reduces, and sperm quantity reduces, vigor descends, and teratospermia increases.
Vitamin A is a fatsoluble vitamin, is soluble in organic solvent and fat, and is water insoluble.Because the fusing point of vitamin A is higher than the temperature of animal body, therefore, vitamin A exists with solid form in animal body, the speed of its absorption rate and vitamin A crystal big or small closely related, crystal particle diameter greatly then absorbs slowly, and absorbance is low, otherwise crystal particle diameter is more little, absorbs fast more, abundant more.
Because it is all perishable that vitamin A is met heat, light, acid etc., could use so generally need be made into microcapsule.Type vitamin A microcapsulesization normally earlier with the vitamin A crystallization or join oil with the aqueous solution that contains protecting colloid heat, emulsifying, again with the emulsion spray drying, or, obtain through fluidized drying again emulsion elder generation mist projection granulating.
Chinese patent CN1965657 (A) has introduced a kind of method for preparing type vitamin A microcapsules, this method joins vitamin A oil in the modified starch solution that prepared in advance before several hours, high speed dispersion emulsifying under 5000～20000rpm rotating speed, be homogenizing twice under 10～40MPa at room temperature, homogenization pressure then, last centrifugal spray drying obtains type vitamin A microcapsules.
Chinese patent CN101214219A has then reported the method for preparing vitamin A, Vitamin E contained micro capsule, used the high speed shear under 10000～20500rpm rotating speed in its emulsion process, and homogenizing is 3 times under 40～60MPa, and then spray drying prepares microcapsule.
The above-mentioned high speed shear emulsifying problem that method that homogenizing prepares type vitamin A microcapsules is difficult to overcome below existing that adds high pressure:
1) emulsion process is carried out in batches, and single batch of emulsification times is long, and the emulsifying temperature height easily causes vitamin A rotten;
2) high-speed shearing machine and high pressure homogenize acc power are big, the energy consumption height, and the localized hyperthermia that shears the position generation is difficult to control, also easily causes vitamin A rotten;
3) owing to batch operation, the intact back of emulsifying is when spray drying, and the easy layering of emulsion cause unstable product quality, and accumulative vitamin A oil droplet becomes big crystal grain in product, thereby influences the bioavailability of product;
4) existing emulsification method is difficult to make vitamin A to be scattered in the microcapsule with nano-grade size, thereby has had influence on the use in some products.
Summary of the invention
The objective of the invention is deficiency, a kind of type vitamin A microcapsules preparation method of the nano-dispersed that can be continuously produced is provided at existing type vitamin A microcapsules production technology.
The preparation method of serialization nanometer dispersed vitamin A microcapsule may further comprise the steps:
1) with vitamin A crystallization, antioxidant, solvent together in grinder 0～20 ℃ be ground to vitamin A crystallization particle diameter 2～5 μ m, obtain content and be 5～10% vitamin A dispersion liquid;
2) gelatin, isinglass or modified starch is soluble in water, be made into 10～20% protecting colloid aqueous solutions, be chilled to 15～25 ℃;
3) the vitamin A dispersion liquid is warming up to 60～65 ℃ with pump through the coil pipe preheater, be incubated 3～5 minutes, after treating vitamin A dissolving fully, be cooled to 15～25 ℃ through coiled pipe cooler again, send into then in the hypergravity RPB crystallize device that has liquid distribution trough, simultaneously, with protecting colloid solution with being pumped in the same hypergravity RPB crystallize device, vitamin A is separated out with the nanoscale crystal form, obtain the vitamin A dispersion liquid of nano-dispersed in outlet;
4) the vitamin A dispersion liquid of nano-dispersed is packed into carry out spray drying in the spray dryer, promptly obtain the type vitamin A microcapsules of nano-dispersed, the tail gas of spray dryer absorbs through water, distills recyclable solvent.
Described antioxidant is ethoxy quinoline, tocopherol, 2,6 ditertiary butyl p cresol or butylhydroxy anisole.Solvent is ethanol, isopropyl alcohol or acetone.The weight ratio of vitamin A dispersion liquid and protecting colloid aqueous solution is 1: 3～9.Hypergravity RPB crystallize device has liquid distribution trough, and filler is a metal gauze, and rotating speed is 1000～3000 rev/mins.Spray dryer has the fluidization chiller.
Core of the present invention is that the effect by hypergravity in hypergravity RPB crystallize device makes vitamin A separate out with the crystal form of nano-grade size with vitamin A solution and protecting colloid aqueous solution, thereby forms the vitamin A dispersion liquid of nano-dispersed; Lower temperature then can make the vitamin A of separating out keep solid-state, thereby has avoided coalescence again; Directly can avoid in the microcapsule vitamin A because of the phenomenon of fusing coalescence equally after the spray drying with the fluidization cooling.Because hypergravity RPB crystallize device is continued operation, thereby technology of the present invention can serialization prepares the type vitamin A microcapsules of nano-dispersed.
But advantage of the present invention is a continuous production, and the vitamin A crystal particle diameter is little in the product, and product is widely applicable, the bioavailability height.
The specific embodiment
Below in conjunction with embodiment the present invention is described in detail.
Embodiment 1
The crystallization of 100kg vitamin A is ground to vitamin A crystallization particle diameter 5 μ ms under 20 ℃ of the temperature with 1898kg ethanol, 2kg ethoxy quinoline in sand mill, obtains content and be 5% vitamin A dispersion liquid.
The 1000kg gelatin is dissolved in the 9000kg water, is made into 10% aqueous gelatin solution, be cooled to 25 ℃ standby.
Said vitamin A dispersion liquid is warming up to 65 ℃ with 100kg/ hour flow through coil pipe to preheater with pump, be incubated 5 minutes, after treating that vitamin A dissolves fully, be cooled to 25 ℃ through coiled pipe cooler again, send into then that to have liquid distribution trough, rotating speed be in 1000 rev/mins the hypergravity RPB crystallize device, simultaneously, aqueous gelatin solution is sent in the same hypergravity RPB crystallize device with 500kg/ hour flow with pump, vitamin A is separated out with the nano-scale crystal form, obtain the vitamin A dispersion liquid of nano-dispersed in outlet.Said vitamin A dispersion liquid sent into carry out spray drying in the spray dryer that has the fluidization chiller, promptly to obtain the type vitamin A microcapsules that temperature is lower than 30 ℃ nano-dispersed in 54kg/ hour.Spray dryer tail gas is after secondary water absorption tower absorbs, and absorbing the water continuous still can obtain 95% ethanol by 92kg/ hour flow.After 20 hours altogether the type vitamin A microcapsules of 1080kg nano-dispersed.By analysis, vitamin A content is 9.0% in the microcapsule, and granularmetric analysis shows the D of vitamin A crystal in the product
95Be 205nm.
Embodiment 2
The crystallization of 100kg vitamin A is lower than with 898kg isopropyl alcohol, 2kg tocopherol temperature in sand mill is ground to vitamin A crystallization particle diameter 2 μ m under 0 ℃, obtain content and be 10% vitamin A dispersion liquid.
The 450kg isinglass is dissolved in the 1800kg water, is made into 15% isinglass aqueous solution, be cooled to 15 ℃ standby.
Said vitamin A dispersion liquid is warming up to 60 ℃ with 100kg/ hour flow through coil pipe to preheater with pump, be incubated 3 minutes, after treating that vitamin A dissolves fully, be cooled to 15 ℃ through coiled pipe cooler again, send into then that to have liquid distribution trough, rotating speed be in 1500 rev/mins the hypergravity RPB crystallize device, simultaneously, the isinglass aqueous solution is sent in the same hypergravity RPB crystallize device with 300kg/ hour flow with pump, vitamin A is separated out with the nano-scale crystal form, obtain the vitamin A dispersion liquid of nano-dispersed in outlet.Said vitamin A dispersion liquid sent into carry out spray drying in the spray dryer that has the fluidization chiller, promptly to obtain the type vitamin A microcapsules that temperature is lower than 30 ℃ nano-dispersed in 54kg/ hour.Spray dryer tail gas is after secondary water absorption tower absorbs, and absorbing the water continuous still can obtain 87% isopropyl alcohol by 91kg/ hour flow.After 10 hours altogether the type vitamin A microcapsules of 540kg nano-dispersed.By analysis, vitamin A content is 17.7% in the microcapsule, and granularmetric analysis shows the D of vitamin A crystal in the product
95Be 230nm.
Embodiment 3
The crystallization of 100kg vitamin A is lower than with 898kg acetone, 1kgBHT, 1kgBHA temperature in sand mill is ground to vitamin A crystallization particle diameter 4 μ m under 10 ℃, obtain content and be 10% vitamin A dispersion liquid.
The 1800kg modified starch is dissolved in the 7200kg water, is made into 20% modified starch aqueous solution, be cooled to 20 ℃ standby.
Said vitamin A dispersion liquid is warming up to 62 ℃ with S0kg/ hour flow through coil pipe to preheater with pump, be incubated 4 minutes, after treating that vitamin A dissolves fully, be cooled to 20 ℃ through coiled pipe cooler again, send into then that to have liquid distribution trough, rotating speed be in 3000 rev/mins the hypergravity RPB crystallize device, simultaneously, the modified starch aqueous solution is sent in the same hypergravity RPB crystallize device with 450kg/ hour flow with pump, vitamin A is separated out with the nano-scale crystal form, obtain the vitamin A dispersion liquid of nano-dispersed in outlet.Said vitamin A dispersion liquid sent into carry out spray drying in the spray dryer that has the fluidization chiller, promptly to obtain the type vitamin A microcapsules that temperature is lower than 30 ℃ nano-dispersed in 93kg/ hour.Spray dryer tail gas is after secondary water absorption tower absorbs, and absorbing the water continuous still can obtain 98% acetone by 45kg/ hour flow.After 20 hours altogether the type vitamin A microcapsules of 1860kg nano-dispersed.By analysis, vitamin A content is 5.1% in the microcapsule, and granularmetric analysis shows the D of vitamin A crystal in the product
95Be 210nm.
Claims (4)
1. the preparation method of a serialization nanometer dispersed vitamin A microcapsule is characterized in that may further comprise the steps:
1) with vitamin A crystallization, antioxidant, solvent together in grinder 0～20 ℃ be ground to vitamin A crystallization particle diameter 2～5 μ m, obtain content and be 5～10% vitamin A dispersion liquid;
2) gelatin, isinglass or modified starch is soluble in water, be made into 10～20% protecting colloid aqueous solutions, be chilled to 15～25 ℃;
3) the vitamin A dispersion liquid is warming up to 60～65 ℃ with pump through the coil pipe preheater, be incubated 3～5 minutes, after treating vitamin A dissolving fully, be cooled to 15～25 ℃ through coiled pipe cooler again, send into then in the hypergravity RPB crystallize device that has liquid distribution trough, simultaneously, with protecting colloid solution with being pumped in the same hypergravity RPB crystallize device, vitamin A is separated out with the nanoscale crystal form, obtain the vitamin A dispersion liquid of nano-dispersed in outlet;
4) the vitamin A dispersion liquid of nano-dispersed is squeezed into carried out spray drying in the spray dryer, promptly obtain the type vitamin A microcapsules of nano-dispersed, the tail gas of spray dryer absorbs through water, distills recyclable solvent;
Described solvent is ethanol, isopropyl alcohol or acetone; Described spray dryer has the fluidization chiller.
2. the preparation method of serialization nanometer dispersed vitamin A microcapsule according to claim 1 is characterized in that described antioxidant is ethoxy quinoline, tocopherol, 2,6 ditertiary butyl p cresol or butylhydroxy anisole.
3. the preparation method of serialization nanometer dispersed vitamin A microcapsule according to claim 1, the weight ratio that it is characterized in that described vitamin A dispersion liquid and protecting colloid aqueous solution is 1: 3～9.
4. the preparation method of serialization nanometer dispersed vitamin A microcapsule according to claim 1 is characterized in that described hypergravity RPB crystallize device has liquid distribution trough, and filler is a metal gauze, and rotating speed is 1000～3000 rev/mins.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104522681A (en) * | 2015-01-10 | 2015-04-22 | 黄家亨 | Vitamin A absorption promoter and corresponding vitamin A replenisher comprising same |
| WO2023135583A1 (en) * | 2022-01-17 | 2023-07-20 | Fondazione Istituto Italiano Di Tecnologia | Vitamin nanoclusters as therapeutic and nutraceutic agents and carriers |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101744790B (en) * | 2010-01-22 | 2012-06-06 | 浙江大学 | Method for preparing stable-type vitamin A microcapsules continuously |
| CN101803741B (en) * | 2010-04-20 | 2012-05-02 | 浙江新和成股份有限公司 | Method for preparing nano vitamin E water dispersing powder preparation by using supergravity method |
| US9173818B2 (en) | 2011-03-25 | 2015-11-03 | Zhejiang Nhu Company Ltd | Method for preparing stable-type vitamin A microcapsules continuously |
| CN102362864B (en) * | 2011-10-26 | 2013-03-13 | 浙江新维普添加剂有限公司 | Method for raising free-flowing property and bulk density of vitamin A or vitamin D3 microcapsules |
| CN104351473B (en) * | 2014-10-22 | 2018-02-02 | 刘希悦 | A kind of preparation method of Aquavite micropill for livestock and poultry |
| CN107594597B (en) * | 2017-07-31 | 2020-05-12 | 浙江新和成股份有限公司 | Fat-soluble nutrient microcapsule and preparation method thereof |
| CN114653314B (en) * | 2020-12-23 | 2022-11-25 | 北京化工大学 | Method for preparing self-assembly type microcapsule |
| CN114315675B (en) * | 2022-01-05 | 2024-02-02 | 万华化学集团股份有限公司 | Preparation of hot water insoluble vitamin A acetate particles |
| CN116161688A (en) * | 2022-12-12 | 2023-05-26 | 雅安百图高新材料股份有限公司 | Preparation method of nano spherical alumina |
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| CN1391467A (en) * | 1999-11-17 | 2003-01-15 | 泰谷生物技术有限公司 | Method of microencapsulation |
| CN1451648A (en) * | 2003-04-29 | 2003-10-29 | 北京化工大学 | Process for preparing micropowdered salbutamol sulfate |
| CN1965657A (en) * | 2006-11-27 | 2007-05-23 | 江南大学 | Method for preparing flour nutrition intensifying Vitamin A microcapsule |
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2009
- 2009-03-30 CN CN2009100970647A patent/CN101513394B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1391467A (en) * | 1999-11-17 | 2003-01-15 | 泰谷生物技术有限公司 | Method of microencapsulation |
| CN1451648A (en) * | 2003-04-29 | 2003-10-29 | 北京化工大学 | Process for preparing micropowdered salbutamol sulfate |
| CN1965657A (en) * | 2006-11-27 | 2007-05-23 | 江南大学 | Method for preparing flour nutrition intensifying Vitamin A microcapsule |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104522681A (en) * | 2015-01-10 | 2015-04-22 | 黄家亨 | Vitamin A absorption promoter and corresponding vitamin A replenisher comprising same |
| CN104522681B (en) * | 2015-01-10 | 2016-08-24 | 漯河医学高等专科学校 | A kind of vitamin A absorption accelerator and corresponding vitamin A supplement thereof |
| WO2023135583A1 (en) * | 2022-01-17 | 2023-07-20 | Fondazione Istituto Italiano Di Tecnologia | Vitamin nanoclusters as therapeutic and nutraceutic agents and carriers |
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| CN101513394A (en) | 2009-08-26 |
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