CN102362864A - Method for raising free-flowing property and bulk density of vitamin A or vitamin D3 microcapsules - Google Patents
Method for raising free-flowing property and bulk density of vitamin A or vitamin D3 microcapsules Download PDFInfo
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Abstract
The invention discloses a method for raising the free-flowing property and bulk density of vitamin A or vitamin D3 microcapsules, comprising the following processes: preparing vitamin A or vitamin D3 crystals and anti-oxidant under the protection of nitrogen in proportion in a melting kettle at the temperature of 60-70 DEG C into vitamin A or vitamin D3 melted oil; dissolving Arabic gum, gelatin or modified starch in water of 60-70 DEG C to prepare 30-50% of a protective colloid aqueous solution, removing bubbles at minus 0.05-0.07Mpa and filling nitrogen gas for protection; allowing the above melted oil and the protective colloid aqueous solution to undergo high-speed shearing or emulsification by a high gravity rotating packed bed under the protection of nitrogen gas so as to prepare an emulsion, allowing the emulsion to pass through a film continuous bubble removing device at minus 0.06-minus 0.08Mpa and at 50-65 DEG C so as to remove most tiny bubbles, carrying out spray granulation in a starch bed, and carrying out fluidization desiccation until the moisture is qualified so as to obtain the vitamin A or vitamin D3 microcapsules with good free-flowing property and high bulk density.
Description
Technical field
The present invention relates to a kind of method that improves vitamin A or vitamin D3 microcapsule free-running property and bulk density.
Background technology
Vitamin A and vitamin D3 all are fatsoluble vitamiies, are soluble in organic solvent and fat, and be water insoluble, and it is all perishable to meet light, heat, oxygen, therefore generally is made into microcapsule powder and uses.
As the micro encapsulation embedding techniques; Generally be with after mixing as the vitamin A of core or vitamin D3 fusing back and polymer substance solution as the wall material; Through forming emulsion after high speed shear or the emulsifying of hypergravity RPB; Through mist projection granulating, drying or direct spray drying, obtain the microcapsule finished product at last again.
Through the vitamin A or the vitamin D3 microcapsule product of method for preparing, two important indicators of free-running property and bulk density are arranged all.As free-running property too missionary society in follow-up use, produce be stained with sticking, lump, be not easy and the blended problem of other products; Problems such as more storages and transport space are more packed, taken to the too little product needed that then in follow-up use, produces waft dust, equal in quality of bulk density.Therefore, the too low meeting of free-running property difference and bulk density is used the user and is produced inconvenience, improves use cost simultaneously.
Patent CN1965657 (A) has introduced a kind of method for preparing of flour nutrition intensifying Vitamin A microcapsule; This method is the wall material with octenyl succinate HI-CAP100; With the vitamin A oil was core, at 5000-20000 rev/min of following high speed dispersion 1-2 minute.And then homogenizing 2 times under the 10-40MPa, last spray drying prepares microcapsule.
Patent CN101214219 (A) has introduced the method for preparing for preparing the nano-sphere/microsphere double-embedding system of vitamin A, vitamin E; Used the high speed shear of 1000-20500rpm in its emulsion process; Homogenizing three times under the 40-60MP again, then spray drying prepares microcapsule.
Patent CN101744790 (A) has introduced a kind of method for preparing of stable-type vitamin A microcapsules continuously; Under nitrogen protection; Vitamin A crystal and antioxidant are made into the vitamin A melting oil that contains antioxidant; With being pumped in the hypergravity RPB emulsator that has liquid distribution trough; But the aqueous solution that will contain the gelation modified starch simultaneously with being pumped into above-mentioned hypergravity RPB emulsator, obtains the vitamin A emulsion after deoxidation treatment, spray drying obtains type vitamin A microcapsules.
The free-running property of all not mentioned gained microcapsule product and bulk density problem in the described microcapsule preparation method of above-mentioned Patent data.
The above-mentioned microcapsule that is prepared into through high speed shear or the emulsifying of hypergravity RPB is cut into slices; Find through the sem observation analysis; All contain a large amount of micro-bubbles even big cavity in microcapsule inside; Microcapsule also becomes irregular sphere because of the influence in these bubbles and cavity, thereby influences the free-running property and the bulk density of product.
The inventor has mentioned the deoxygenation under vacuum of modified starch aqueous solution at CN101744790 (A), but this invention does not still solve the air bubble problem in the microcapsule.
Summary of the invention
The objective of the invention is provides a kind of method that improves vitamin A or vitamin D3 microcapsule free-running property and bulk density to the deficiency in existing vitamin A and the vitamin D3 microencapsulation process.
The method that improves vitamin A or vitamin D3 microcapsule free-running property and bulk density may further comprise the steps:
(1) under nitrogen protection, vitamin A crystallization or vitamin D3 crystallization and antioxidant are added in the melting kettle by weight the ratio that is 100:0.5 ~ 5, in 60 ~ 70 ℃ of fusings down, be made into the molten oil of vitamin A melting oil or vitamin D3;
(2) arabic gum, gelatin or modified starch are dissolved in 60 ~ 70 ℃ the water ,-0.05 ~-remove bubble under the 0.07Mpa condition after the inflated with nitrogen protection, obtain weight ratio and be 30 ~ 50% protecting colloid aqueous solution;
(3) with the molten oil of vitamin A melting oil or vitamin D3 and above-mentioned weight ratio be 30 ~ 50% protecting colloid aqueous solution,, obtain emulsion through high speed shear or the emulsifying of hypergravity RPB;
(4) above-mentioned emulsion is removed air bubble apparatus continuously through thin film; In-0.06 ~-in starch bed, carry out mist projection granulating after removing the micro-bubble in the emulsion under the 0.08Mpa, 50 ~ 65 ℃ of conditions; Through fluidized drying, obtain type vitamin A microcapsules or vitamin D3 microcapsule then.
Described antioxidant is tocopherol or sodium L-ascorbate-2-phosphate.
Advantage of the present invention is: remove temperature in the air bubble apparatus, vacuum or the emulsion time of staying continuously through regulating thin film, can most micro-bubbles be removed, thereby improve vitamin A or vitamin D3 microcapsule product free-running property and bulk density.
Description of drawings
Fig. 1 is that thin film used in the present invention removes air bubble apparatus continuously;
Fig. 2 is embodiment 1 a products obtained therefrom electron micrograph outside drawing;
Fig. 3 is embodiment 1 a products obtained therefrom electron micrograph profile;
Fig. 4 is comparative example 1 a products obtained therefrom electron micrograph outside drawing;
Fig. 5 is comparative example 1 a products obtained therefrom electron micrograph profile;
Fig. 6 is comparative example 1 a products obtained therefrom electron micrograph profile;
Fig. 7 is embodiment 2 products obtained therefrom electron micrograph outside drawings;
Fig. 8 is embodiment 2 products obtained therefrom electron micrograph profiles;
Fig. 9 is comparative example 2 products obtained therefrom electron micrograph outside drawings;
Figure 10 is comparative example 2 products obtained therefrom electron micrograph profiles;
Figure 11 is comparative example 2 products obtained therefrom electron micrograph profiles;
Figure 12 is embodiment 3 products obtained therefrom electron micrograph outside drawings;
Figure 13 is embodiment 3 products obtained therefrom electron micrograph profiles;
Figure 14 is comparative example 3 products obtained therefrom electron micrograph outside drawings;
Figure 15 is comparative example 3 products obtained therefrom electron micrograph profiles;
Figure 16 is comparative example 3 products obtained therefrom electron micrograph profiles.
The specific embodiment
As shown in Figure 1, thin film used in the present invention removes air bubble apparatus continuously and comprises mashing pump 1, observation window 2, vacuum pump 3, air bleeding valve 4, liquid distribution trough 5, material inlet 6, thermostatted water outlet 7, guiding gutter 8, thermostatted water import 9.Device body top is provided with observation window 2, vacuum pump 3, air bleeding valve 4, and the device body bottom is provided with material pump 1, liquid distribution trough 5, material inlet 6, thermostatted water outlet 7, guiding gutter 8, thermostatted water import 9.
The method that improves vitamin A or vitamin D3 microcapsule free-running property and bulk density may further comprise the steps:
(1) under nitrogen protection, vitamin A crystallization or vitamin D3 crystallization and antioxidant are added in the melting kettle by weight the ratio that is 100:0.5 ~ 5, in 60 ~ 70 ℃ of fusings down, be made into the molten oil of vitamin A melting oil or vitamin D3;
(2) arabic gum, gelatin or modified starch are dissolved in 60 ~ 70 ℃ the water ,-0.05 ~-remove bubble under the 0.07Mpa condition after the inflated with nitrogen protection, obtain weight ratio and be 30 ~ 50% protecting colloid aqueous solution;
(3) with the molten oil of vitamin A melting oil or vitamin D3 and above-mentioned weight ratio be 30 ~ 50% protecting colloid aqueous solution,, obtain emulsion through high speed shear or the emulsifying of hypergravity RPB;
(4) above-mentioned emulsion is removed air bubble apparatus continuously through thin film as shown in Figure 1; In-0.06 ~-in starch bed, carry out mist projection granulating after removing the micro-bubble in the emulsion under the 0.08Mpa, 50 ~ 65 ℃ of conditions; Through fluidized drying, obtain type vitamin A microcapsules or vitamin D3 microcapsule then.
Described antioxidant is tocopherol or sodium L-ascorbate-2-phosphate.
Below will specify the present invention through embodiment.
Embodiment 1
Under nitrogen protection, the crystallization of double centner vitamin A and 0.5 kilogram of tocopherol are melted down in 60 ℃, be made into vitamin A melting oil.Simultaneously, 200 kilograms of arabic gums be dissolved in 300 kilograms of 60 ℃ of water be made into 40% arabic gum aqueous solution, under-0.07MPa, remove bubble after the inflated with nitrogen protection.
Under the high speed shear condition, vitamin A melting oil slowly is added drop-wise in the above-mentioned arabic gum aqueous solution and carries out emulsifying, be prepared into the vitamin A emulsion.
Said vitamin A emulsion is removed air bubble apparatus continuously through thin film, after removing most of micro-bubble under-0.08Mpa, the 50 ℃ of conditions, in starch bed, carry out mist projection granulating, qualified through fluidized drying to moisture then, obtain 335 kilograms of products.
Be 35 ° the angle of repose according to the said method testing product of GB11986-89, and the bulk density of product is 0.73g/cm
3Electron micrograph as shown in Figures 2 and 3, visible by Fig. 2 and Fig. 3, gained type vitamin A microcapsules shape is regular, the section scanning electron microscopic observation has only a small amount of micro-bubble.
Comparative example 1
Under nitrogen protection, the crystallization of double centner vitamin A and 0.5 kilogram of tocopherol are melted down in 60 ℃, be made into vitamin A melting oil.Simultaneously, 200 kilograms of arabic gums are dissolved in 300 kilograms of 60 ℃ of water are made into 40% arabic gum aqueous solution.
Under the high speed shear condition, vitamin A melting oil slowly is added drop-wise to and carries out emulsifying in the arabic gum aqueous solution, be prepared into the vitamin A emulsion.
Said vitamin A emulsion is carried out mist projection granulating in starch bed, qualified through fluidized drying to moisture then, obtain 323 kilograms of products.
Be 45 ° the angle of repose according to the said method testing product of GB11986-89, and the bulk density of product is 0.59g/cm
3Electron micrograph such as Fig. 4, Fig. 5 and shown in Figure 6, visible by Fig. 4, Fig. 5 and Fig. 6, gained type vitamin A microcapsules shape irregularity, the section scanning electron microscopic observation has a large amount of micro-bubbles and big cavity is arranged.
Embodiment 2
Under nitrogen protection, the crystallization of double centner vitamin A and 5 kilograms of sodium L-ascorbate-2-phosphate are melted down in 65 ℃, be made into vitamin A melting oil.200 kilograms of gelatin are dissolved in 200 kilograms of 70 ℃ of water are made into 50% aqueous gelatin solution, inflated with nitrogen protection after removing bubble under the vacuum of-0.05MPa.
Vitamin A melting oil and aqueous gelatin solution are passed through the emulsifying of hypergravity RPB together, be prepared into the vitamin A emulsion.
Said vitamin A emulsion is removed air bubble apparatus continuously through thin film, after removing most of micro-bubble under-0.07Mpa, the 60 ℃ of conditions, in starch bed, carry out mist projection granulating, qualified through fluidized drying to moisture then, obtain 332 kilograms of products.
Be 34 ° the angle of repose according to the said method testing product of GB11986-89, and the bulk density of product is 0.71g/cm
3Electron micrograph such as Fig. 7 and shown in Figure 8, visible by Fig. 7 and Fig. 8, gained type vitamin A microcapsules shape is regular, and the section scanning electron microscopic observation has only a small amount of micro-bubble.
Comparative example 2
Under nitrogen protection, the crystallization of double centner vitamin A and 5 kilograms of sodium L-ascorbate-2-phosphate are melted down in 65 ℃, be made into vitamin A melting oil.200 kilograms of gelatin are dissolved in 200 kilograms of 70 ℃ of water are made into 50% aqueous gelatin solution.
Vitamin A melting oil and aqueous gelatin solution are passed through the emulsifying of hypergravity RPB together, be prepared into the vitamin A emulsion.
Said vitamin A emulsion is carried out mist projection granulating in starch bed, qualified through fluidized drying to moisture then, obtain 321 kilograms of products.
Be 44 ° the angle of repose according to the said method testing product of GB11986-89, and the bulk density of product is 0.58g/cm
3Electron micrograph such as Fig. 9, Figure 10 and shown in Figure 11, visible by Fig. 9, Figure 10 and Figure 11, gained type vitamin A microcapsules shape irregularity, the section scanning electron microscopic observation has a large amount of micro-bubbles and big cavity is arranged.
Embodiment 3
Under nitrogen protection, 20 kilograms of vitamin D3 crystallizations and 0.4 kilogram of tocopherol are melted under 70 ℃ temperature, be made into the molten oil of vitamin D3.150 kilograms of modified starches are dissolved in 350 kilograms of 65 ℃ of water are made into 30% modified starch aqueous solution, inflated with nitrogen protection after removing bubble under the vacuum of-0.06MPa.
Under the high speed shear condition, the molten oil of vitamin D3 slowly is added drop-wise to and carries out emulsifying in the modified starch aqueous solution, be prepared into the vitamin D3 emulsion.
Said vitamin D3 emulsion is removed air bubble apparatus continuously through thin film, after removing most of micro-bubble under-0.06Mpa, the 65 ℃ of conditions, in starch bed, carry out mist projection granulating, qualified through fluidized drying to moisture then, obtain product 183 kilograms of product.
According to GB11986-89, be 33 ° the angle of repose of testing product, and the bulk density of product is 0.76g/cm
3Electron micrograph such as Figure 12 and shown in Figure 13, visible by Figure 12 and Figure 13, gained vitamin D3 microcapsule shape is regular, and the section scanning electron microscopic observation does not have micro-bubble.
Comparative example 3
Under nitrogen protection, 20 kilograms of vitamin D3 crystallizations and 0.4 kilogram of tocopherol are melted under 70 ℃ temperature, be made into the molten oil of vitamin D3.150 kilograms of modified starches are dissolved in 350 kilograms of 65 ℃ of water are made into 30% modified starch aqueous solution.
Under the high speed shear condition, the molten oil of vitamin D3 slowly is added drop-wise to and carries out emulsifying in the modified starch aqueous solution, be prepared into the vitamin D3 emulsion.
Said vitamin D3 emulsion is carried out mist projection granulating in starch bed, qualified through fluidized drying to moisture then, obtain 181 kilograms of products.
According to GB11986-89, be 48 ° the angle of repose of testing product, and the bulk density of product is 0.63g/cm
3Electron micrograph such as Figure 14, Figure 15 and shown in Figure 16, visible by Figure 14, Figure 15 and Figure 16, gained vitamin D3 microcapsule shape irregularity, the section scanning electron microscopic observation has a large amount of micro-bubbles and big cavity is arranged.
Claims (2)
1. method that improves vitamin A or vitamin D3 microcapsule free-running property and bulk density is characterized in that may further comprise the steps:
(1) under nitrogen protection, vitamin A crystallization or vitamin D3 crystallization and antioxidant are added in the melting kettle by weight the ratio that is 100:0.5 ~ 5, in 60 ~ 70 ℃ of fusings down, be made into the molten oil of vitamin A melting oil or vitamin D3;
(2) arabic gum, gelatin or modified starch are dissolved in 60 ~ 70 ℃ the water ,-0.05 ~-remove bubble under the 0.07Mpa condition after the inflated with nitrogen protection, obtain weight ratio and be 30 ~ 50% protecting colloid aqueous solution;
(3) with the molten oil of vitamin A melting oil or vitamin D3 and above-mentioned weight ratio be 30 ~ 50% protecting colloid aqueous solution,, obtain emulsion through high speed shear or the emulsifying of hypergravity RPB;
(4) above-mentioned emulsion is removed air bubble apparatus continuously through thin film; In-0.06 ~-in starch bed, carry out mist projection granulating after removing the micro-bubble in the emulsion under the 0.08Mpa, 50 ~ 65 ℃ of conditions; Through fluidized drying, obtain type vitamin A microcapsules or vitamin D3 microcapsule then.
2. a kind of method that improves vitamin A or vitamin D3 microcapsule free-running property and bulk density according to claim 1 is characterized in that described antioxidant is tocopherol or sodium L-ascorbate-2-phosphate.
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| CN104351473A (en) * | 2014-10-22 | 2015-02-18 | 浙江万方生物科技有限公司 | Preparation method of water-soluble multivitamin micropills for livestock and poultry |
| US20180207277A1 (en) * | 2017-01-20 | 2018-07-26 | Zhejiang Medicine Co., Ltd. Xinchang Pharmaceutical Factory | Stable Fat-soluble Active Ingredient Composition, Microcapsule and Process Of Preparation and Use Thereof |
| CN108324699A (en) * | 2017-01-20 | 2018-07-27 | 浙江医药股份有限公司新昌制药厂 | Stable fat-soluble active ingredient composition, micro-capsule and its preparation method and application |
| CN109674062A (en) * | 2019-02-01 | 2019-04-26 | 浙江花园营养科技有限公司 | A kind of preparation method of stability vitamine D3 nano freeze-dried powder |
| CN110250521A (en) * | 2019-05-15 | 2019-09-20 | 万华化学集团股份有限公司 | A kind of preparation method of retinyl acetate microcapsules |
| WO2020132773A1 (en) * | 2018-12-27 | 2020-07-02 | Universidad De Santiago De Chile | Material that incorporates vitamin d for the subsequent release thereof and method for obtaining the material |
| CN113317427A (en) * | 2021-05-31 | 2021-08-31 | 晨光生物科技集团股份有限公司 | Lutein ester preparation for tabletting and preparation method thereof |
| CN114365847A (en) * | 2022-01-18 | 2022-04-19 | 杭州民生健康药业股份有限公司 | High-stability multiple inclusion microcapsule powder, preparation method thereof and vitamin capsule |
| CN114586984A (en) * | 2020-12-07 | 2022-06-07 | 万华化学集团股份有限公司 | Method for continuously preparing vitamin A microcapsules |
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| CN104351473A (en) * | 2014-10-22 | 2015-02-18 | 浙江万方生物科技有限公司 | Preparation method of water-soluble multivitamin micropills for livestock and poultry |
| CN104351473B (en) * | 2014-10-22 | 2018-02-02 | 刘希悦 | A kind of preparation method of Aquavite micropill for livestock and poultry |
| AU2018208993B2 (en) * | 2017-01-20 | 2021-07-08 | Zhejiang Medicine Co., Ltd. Vitamin Factory | Stable and liposoluble active ingredient composition, microcapsule, and preparation method and application thereof |
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| WO2020132773A1 (en) * | 2018-12-27 | 2020-07-02 | Universidad De Santiago De Chile | Material that incorporates vitamin d for the subsequent release thereof and method for obtaining the material |
| CN109674062A (en) * | 2019-02-01 | 2019-04-26 | 浙江花园营养科技有限公司 | A kind of preparation method of stability vitamine D3 nano freeze-dried powder |
| CN110250521A (en) * | 2019-05-15 | 2019-09-20 | 万华化学集团股份有限公司 | A kind of preparation method of retinyl acetate microcapsules |
| CN114586984A (en) * | 2020-12-07 | 2022-06-07 | 万华化学集团股份有限公司 | Method for continuously preparing vitamin A microcapsules |
| CN114586984B (en) * | 2020-12-07 | 2023-12-19 | 万华化学集团股份有限公司 | Method for continuously preparing vitamin A microcapsules |
| CN113317427A (en) * | 2021-05-31 | 2021-08-31 | 晨光生物科技集团股份有限公司 | Lutein ester preparation for tabletting and preparation method thereof |
| CN114365847A (en) * | 2022-01-18 | 2022-04-19 | 杭州民生健康药业股份有限公司 | High-stability multiple inclusion microcapsule powder, preparation method thereof and vitamin capsule |
| CN114365847B (en) * | 2022-01-18 | 2023-09-22 | 杭州民生健康药业股份有限公司 | High-stability multi-inclusion microcapsule powder, preparation method thereof and vitamin capsule |
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