Method for granulating, forming, and drying fat soluble nutrient microcapsule particles

10821412 ยท 2020-11-03

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Abstract

The present invention provides a method for drying high-stability microcapsule particles containing multiple double bonds fat soluble nutrients comprises: a) preparing a microcapsule emulsion containing multiple double bonds fat soluble nutrients, performing spray granulation on the microcapsule emulsion in a spray system (1), and meanwhile blasting air into the spray system (1), the blasted air wrapping adsorption materials, and the microcapsule emulsion being immediately solidified and sized after coming into contact with the air, so as to obtain liquid droplets having surfaces to which adsorption materials are adsorbed; b) performing fluidized drying on the liquid droplets having surfaces to which the adsorption materials are adsorbed in the step a) in a multi-stage fluidized bed system (5); c) collecting non-adsorbed adsorption materials by means of an adsorption material dust removal, recovery and circulation system; and d) collecting microcapsule particle products.

Claims

1. A method for drying microcapsule particles containing multiple double bonds fat soluble nutrients, comprising the following steps: a) preparing a microcapsule emulsion containing multiple double bonds fat soluble nutrients, performing spray granulation on the microcapsule emulsion in a spray system at a temperature of 10-90 C., and meanwhile blasting air into the spray system, the blasted air wrapping adsorption materials, and the microcapsule emulsion being immediately solidified and sized after coming into contact with the air, so as to obtain liquid droplets having surfaces to which adsorption materials are adsorbed; b) performing fluidized drying on the liquid droplets having surfaces to which the adsorption material is adsorbed in the step a) in a multi-stage fluidized bed system, wherein the number of stages of the multi-stage fluidized bed system is 1-4 level, the differential pressure between two adjacent stages of the multi-stage fluidized bed systems is 20 psi; the inlet air temperature of the multi-stage fluidized bed system is in a range of 20-120 C.; the inlet air temperature of a lower fluidized bed is higher than that of an upper fluidized bed, and the inlet air temperature difference is 20-40 C.; c) collecting non-adsorbed adsorption materials by means of an adsorption material dust removal, recovery and circulation system; and d) collecting microcapsule particle products.

2. The method according to claim 1, wherein the microcapsule emulsion comprises a fat-soluble nutrient containing multiple unsaturated double bonds and a capsule shell material.

3. The method according to claim 2, wherein the fat-soluble nutrient containing multiple unsaturated double bonds is selected from the group consisting of Vitamin A, Vitamin E, natural Vitamin E, Vitamin D3, coenzyme Q10, reduced coenzyme Q10, curcumin, carotenoids, polyunsaturated fatty acids; the capsule shell material comprises animal capsule shell material and vegetable capsule shell material.

4. The method according to claim 3, wherein the carotenoid is beta-carotene, lutein, astaxanthin, ycopene, and zeaxanthin; the polyunsaturated fatty acid is derived from animal extract oil, fermented source and synthetic source; the polyunsaturated fatty acid comprises conjugated linoleic acid, arachidonic acid, linoleic acid, linolenic acid, EPA, DHA and a mixture thereof; the animal capsule shell material is gelatin; the vegetable capsule shell material is Arabic gum, modified starch, sodium caseinates.

5. The method according to claim 1, wherein the adsorption material comprises modified starches, silicon dioxide, phosphorus calcium silicate and phosphorus aluminum silicate.

6. The method according to claim 1, wherein in step b), a fluidized drying time of the multi-stage fluidized bed system is within 4.0 hours.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) FIG. 1 shows a spray drying flow diagram of a multi-stage fluidized bed system of the present invention;

(2) FIG. 2 shows a spray drying flow diagram of a multi-stage fluidized bed system of the prior art.

DETAILED DESCRIPTION AND PREFERRED EMBODIMENTS THEREOF

(3) Hereafter, the present invention will be described specifically with reference to the examples. The examples are given only for illustration of the technical solution of the present invention and should not be construed to limit the present invention.

Example 1

(4) 700 g fish oil -3 fatty acid ethyl ester emulsion (EPA 33.5%, DHA 23.1%, total content -3 fatty acid 59.8%) prepared, with 50% solid content, and modified starch (sodium octenyl succinate) as a capsule shell material, are added into a spray granulation system 1 through a liquid material inlet 13 of FIG. 1, to form droplets by atomization of a centrifugal nozzle 12; at the same time, blast cold air (20 C.) from a middle 15 of a spray granulation tower, the blasted air rapping modified starch (aluminum octenyl succinate), and the droplets are solidified immediately when the droplets meet cold air, and fell into the fluidized bed system 5 through the pipe 14.

(5) The fluidized bed system comprises four stages 51, 52, 53 and 54, has corresponding air inlets 512, 522, 532, 542 and induced air inlets 511, 521, 531, 541, controlling the inlet air temperature at air inlets 512, 522, 532, 542 to be 30 C., 50 C., 70 C. and 90 C. respectively, and the modified starch brought from a modified starch storage 3 is carried and wrapped by inlet air. A differential pressure of the fluidized beds 51, 52, 53 and 54 is controlled to be 20 psi, decreasing in turn. After 2.5 hours, most of the modified starch (aluminum octenyl succinate) are introduced into the cyclone separator 4 through pipe 43, and Mark 41 is an induced air inlet of the cyclone separator. After gas-solid separation, the starch is introduced into the starch storage warehouse 3 through pipe 42 (at the beginning stage, the modified starch (aluminum octenyl succinate) is introduced into the storage warehouse through pipe 31). The dried fish oil -3 fatty acid ethyl ester microcapsule particles are collected by opening a valve 55. The moisture content of the particle is 5.6%. No obvious colonies are observed in the sample by microbial culture for three days.

(6) The microcapsule particles obtained are placed in a jar with an electronic nose, to determine odor with a reading of 23.5, and the jar is incubated in a water bath at 60 C. for 10 min, then measure odor by an electronic nose with a reading of 27.6, and the odor change is not significant.

Comparative Example 2

(7) 680 g fish oil -3 fatty acid ethyl ester emulsion (EPA 33.5%, DHA 23.1%, total content -3 fatty acid 59.8%) prepared, with 50% solid content, and modified starch (sodium octenyl succinate) as a capsule shell material, are added into a spray granulation system 1 through a liquid material inlet 13 of FIG. 2, to form droplets by atomization of a centrifugal nozzle 12; at the same time, blast cold air (20 C.) from a middle 15 of a spray granulation tower, the blasted air wrapping modified starch (aluminum octenyl succinate), and the droplets are solidified immediately when the droplets meet cold air, and fell into the fluidized bed system 2 through the pipe 14.

(8) The fluidized bed system is a conventional fluidized bed system. Blow a modified starch (aluminum octenyl succinate) from an inlet air pipe 21 in order to prevent un-dried microcapsule particles from melting due to an excessively high temperature. Gradually raise an air temperature introduced from an inlet air pipe 21, starting at 20 C., and slowly rising to 70 C. after 6 hours, kept for 2.0 hours, then most of the modified starch (aluminum octenyl succinate) is introduced into the cyclone separator 4 through a pipe 23 (a pipe 22 is an outlet of the adsorption materials of less particles fluidized down), and after gas-solid separation, the starch is introduced into a starch storage warehouse 3 through a pipe 42, at the beginning stage, the modified starch such as aluminum octenyl succinate is introduced into the storage warehouse through pipe 31). The dried fish oil -3 fatty acid ethyl ester microcapsule particles are collected by opening a valve 55. The moisture content of the particle is 6.8%. much colonies (unreadable colonies) are observed in the sample by microbial culture for three days.

(9) The microcapsule particles obtained are placed in a jar with an electronic nose, to determine odor with a reading of 143.2, and the jar is incubated in a water bath at 60 C. for 10 min, then measure odor by an electronic nose with a reading of 257.8, and the odor change is very significant.

(10) It may be seen by comparison that using the multi-stage fluidized drying system of Example 1 may adjust a heating rate according to drying degree of microcapsule particles by using a stepped heating-up; meanwhile the adsorption material is gradually removed from different fluidized beds, thereby further accelerate a drying process of the materials. The whole drying process needs only 2.5 hours, the obtained product has little fishy smell, and has good stability. It is important to detect less microbial by microbial culture.

(11) On the contrary, the condensed droplets of the comparative example 2 are treated by a conventional fluidized bed. A temperature rising procedure of the fluidized bed must be very slow in order to make solidified droplets not to be melted and aggregated because of high temperature. And a drying speed of the materials and adsorption materials are further reduced since the adsorption materials cannot be removed timely. A rising temperature time of fluidized bed from 20 C. to 70 C. is 6.0 hours, a drying time is 2.0 hours. So a total time is nearly 8.0 hours. It is more longer than 2.5 hours relative to that of the present invention, and the stability of the final particle product is obviously inferior to the microcapsule products of Example 1. And the final particle product has a obvious fishy smell. Much colonies (unreadable colonies) are observed in the sample and thus it requires an additional sterilization process.

Examples 3-8

(12) The implement objects and related parameters of Examples 38 are listed in Table 2.

(13) TABLE-US-00001 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Types of active Conjugated Curcumin Astaxanthin, Coenzyme Arachidonic VA, Ingredients in Linoleic Acid Lycopene, Q10, Acid (AA), Vitamin E, Microcapsule (CLA), Lutein, Reduced Algae DHA Vitamin D3, Emulsion Linoleic Acid, beta-carotene Coenzyme Natural Linolenic Acid Q10 Vitamin E capsule shell Gum Arabic Gelatin Modified Sodium Modified Gelatin material in Starch Caseinate Starch Microcapsule Emulsion Adsorption Modified Modified Calcium Modified Silicon Aluminium Material Starch Starch Phosphor Starch Dioxide Phosphor Silicate Silicate Inlet Air 45 C. 90 C. 30 C. 90 C. 10 C. 60 C. Temperature of Spray Granulation System Number of 3 2 4 1 4 2 Fluidized Bed Stage Inlet Air 60, 80, 90 60, 120 20, 40, 60, 80 80 30, 50, 80, 90 60, 100 Temperature of Fluidized Bed ( C.) Fluidized Drying 3.0 hr 2.0 hr 3.0 hr 1 hr 4 hr 2.5 hr Time Moisture Content 5.7% 5.6% 5.2% 8.3% 6.5% 7.1% of Final Product (Weight Percentages) Total Number of n.d. n.d. n.d. <350 cfu/g n.d. n.d. Colonies in Final Products

(14) The experiment of the present invention show that the microcapsule product obtained by the drying method of the present invention has not only good stability, but also no bad smell after being placed for a long time due to a short time of heating and fluidization. Moreover, the process time is greatly shortened, and the efficiency of labor is improved.

(15) The present invention is illustrated by the above examples, however, should understand that the present invention is not limited to special instance and implementation scheme described here. These special examples and implementation plans is aimed at helping the person skilled in the art to practice the present invention. The persons skilled in the art is easily from the spirit and scope of the present invention to further improve and perfect, so the present invention only restricts by the content and scope of the claims of the present invention, and its intention to cover all in the alternative solutions and equivalent solutions which included in appendix claim limit within the scope of the invention spirit.