Method for preparing high-absorptivity silica as lutein carrier

Abstract

The invention discloses a preparation method of high-absorptivity silica as lutein carrier. The method includes adding sodium silicate into a synthesis kettle, introducing steam for heating while stirring, adding water, stirring for reaction to obtain a reaction substrate A, and adding sulfuric acid to the reaction substrate A to obtain reaction solution B; simultaneously adding sulfuric acid and sodium silicate into the reaction solution B, performing synthesis reaction for a given period of time, stopping feeding of sodium silicate, adding sulfuric acid only for post-acidification, and aging to obtain dilute slurry D; and filtering the dilute slurry D, washing, slurrying, drying and packaging to obtain silica microspheres as lutein carrier. The invention accurately controls each process so that the prepared high-absorptivity silica as lutein carrier has high adsorption and good dispersibility and flowability after adsorbing lutein.

Claims

1. A method for preparing absorptive silica as lutein carrier, comprising the steps of: (1) adding sodium silicate into a synthesis kettle, introducing steam for heating while stirring, adding water, stirring for reaction to obtain a reaction substrate A, and adding sulfuric acid for pre-acidification until the solution pH is 8.5-10.5 to obtain reaction solution B; (2) simultaneously adding sulfuric acid and sodium silicate into the reaction solution B, and performing synthesis reaction to obtain reaction solution C; (3) adding sulfuric acid only into the reaction solution C, for post-acidification, until the solution pH reaches 3.5-4.0, and aging to obtain dilute slurry D; (4) filtering the dilute slurry D, washing to obtain a filter cake E, transferring to a slurrying machine, and adding a slurry viscosity reducer to obtain slurry F; and (5) drying the slurry F and packaging to obtain absorptive silica microspheres as lutein carrier, wherein: the sodium silicate has a modulus of 3.30-3.60; the slurry viscosity reducer is food-grade organic acid; the organic acid is citric acid; and in step (1): the feeding amount of the sodium silicate is 4.0-8.0 m.sup.3; the concentration of the sodium silicate in the reaction substrate A is 15-20 Baume; the sulfuric acid is water solution of sulfuric acid with a mass fraction of 15-30%; the feeding speed and feeding time of the sulfuric acid are, respectively, 15 m.sup.3/h and 10-30 minutes; the reaction temperature is 30-60° C.; and the stirring speed is 45-80 rpm.

2. The method in claim 1, wherein in step (2): the sulfuric acid is water solution of sulfuric acid with a mass fraction of 93-99%; the feeding speed of the sulfuric acid is 0.6 m.sup.3/h; the feeding speed of the sodium silicate is 4-8 m.sup.3/h; the feeding time of the sulfuric acid and the sodium silicate is 30-60 minutes; and the reaction temperature is 75-95° C.

3. The method in claim 2, wherein in step (3): the sulfuric acid is water solution of sulfuric acid with a mass fraction of 93-99%; the feeding speed of the sulfuric acid is reduced to 50-75% of what is designated in step (2); the feeding time is 30-60 minutes; and the reaction temperature is 75-95° C. and the aging time is 15-30 minutes.

4. The method in claim 1, wherein: the discharged water electrical conductivity of washing water in the washing process is 3.0-8.0 mS/cm; and pH of the filter cake is 6-7.

5. The method in claim 1, wherein in step (5): the drying method involves drying at an atomization rotation speed in a centrifugal drying tower; the centrifugal drying tower has an inlet temperature of 450-550° C., an outlet temperature of 110-150° C. and a pressure of −150-−50 Pa; and the rotation speed of the atomizer is 5,000-9,000 rpm.

6. The method in claim 1, wherein, in step (5), the packaging step is performed by a vacuum packaging machine under −300-−100 Pa.

Description

BRIEF DESCRIPTION OF FIGURES

(1) FIG. 1 is a flowchart visualizing an embodiment of the present invention.

BRIEF DESCRIPTION OF FIGURES

(2) FIG. 1 is a flowchart visualizing an embodiment of the present invention.

DETAILED DESCRIPTION OF THE EMBODIMENTS

(3) Hereinafter, the technical solutions in the embodiments of the present invention will be described clearly and completely in conjunction with FIG. 1 in the embodiments of the present invention. The described embodiments are only part of the embodiments of the present invention, rather than all of them.

Example 1

(4) A preparation method of high-absorptivity silica as lutein carrier includes (1) adding sodium silicate into a synthesis kettle, introducing steam for heating while stirring, adding water, stirring for reaction to obtain a reaction substrate A, and adding sulfuric acid for pre-acidification until the solution pH is 10.0 to obtain reaction solution B; (2) simultaneously adding sulfuric acid and sodium silicate into the reaction solution B, and performing synthesis reaction to obtain reaction solution C; (3) adding sulfuric acid only into the reaction solution C, for post-acidification, until the solution pH reaches 4.0, and aging to obtain dilute slurry D; (4) filtering the dilute slurry D, washing to obtain a filter cake E, transferring to a slurrying machine, and adding a slurry viscosity reducer to obtain slurry F; and (5) drying the slurry F and packaging to obtain silica microspheres as lutein carrier, which is a uniform coarse powder-like silica product.

(5) The sodium silicate in steps (1) and (2) is water solution of sodium silicate with a concentration of 30 Baume, and has a modulus of 3.30.

(6) In step (1), the feeding amount of the sodium silicate is 8.0 m.sup.3, and the concentration of the sodium silicate in the reaction substrate A is 20 Baume; the sulfuric acid is water solution of sulfuric acid with a mass fraction of 30%, and the feeding speed and feeding time of the sulfuric acid are 15 m.sup.3/h and 25 min, respectively; the reaction temperature is 60° C.; and the stirring speed is 72 rpm.

(7) In step (2), the sulfuric acid is water solution of sulfuric acid with a mass fraction of 98%, the feeding speed of the sulfuric acid is 0.6 m.sup.3/h, the feeding speed of the sodium silicate is 8 m.sup.3/h, the feeding time of the sulfuric acid and the sodium silicate is 60 min, and the reaction temperature is 95° C.

(8) In step (3), the sulfuric acid is water solution of sulfuric acid with a mass fraction of 98%, the feeding speed of the sulfuric acid is 0.3 m.sup.3/h, the feeding time is 30 min, the reaction temperature is 95° C. and the aging time is 30 min.

(9) In step (4), the slurry viscosity reducer is citric acid with the feeding amount of 8.0 Kg, pH of the slurry F is 6.5, and the discharged water electrical conductivity of washing water is 3.0 ms/cm.

(10) In step (5), the drying method involves drying at an atomization rotation speed in a centrifugal drying tower; the centrifugal drying tower has an inlet temperature of 500° C., an outlet temperature of 120° C. and a pressure of −100 Pa; the rotation speed of the atomizer is 9,000 rpm; and the packaging step is performed by a vacuum packaging machine under a pressure of −100 Pa.

Example 2

(11) A preparation method of high-absorptivity silica as lutein carrier includes (1) adding sodium silicate into a synthesis kettle, introducing steam for heating while stirring, adding water, stirring for reaction to obtain a reaction substrate A, and adding sulfuric acid for pre-acidification until the solution pH is 10.0 to obtain reaction solution B; (2) simultaneously adding sulfuric acid and sodium silicate into the reaction solution B, and performing synthesis reaction to obtain reaction solution C; (3) adding sulfuric acid only into the reaction solution C, for post-acidification until the solution pH reaches 4.0, and aging to obtain dilute slurry D; (4) filtering the dilute slurry D, washing to obtain a filter cake E, transferring to a slurrying machine, and adding a slurry viscosity reducer to obtain slurry F; and (5) drying the slurry F and packaging to obtain silica microspheres as lutein carrier, which is a uniform coarse powder-like silica product.

(12) The sodium silicate in steps (1) and (2) is water solution of sodium silicate with a concentration of 38 Baume, and has a modulus of 3.60.

(13) In step (1), the feeding amount of the sodium silicate is 8.0 m.sup.3, and the concentration of the sodium silicate in the reaction substrate A is 20 Baume; the sulfuric acid is water solution of sulfuric acid with a mass fraction of 30%, and the feeding speed and feeding time of the sulfuric acid are 15 m.sup.3/h and 25 min, respectively; the reaction temperature is 40° C.; and the stirring speed is 72 rpm.

(14) In step (2), the sulfuric acid is water solution of sulfuric acid with a mass fraction of 98%, the feeding speed of the sulfuric acid is 0.6 m.sup.3/h, the feeding speed of the sodium silicate is 8 m.sup.3/h, the feeding time of the sulfuric acid and the sodium silicate is 60 min, and the reaction temperature is 85° C.

(15) In step (3), the sulfuric acid is water solution of sulfuric acid with a mass fraction of 98%, the feeding speed of the sulfuric acid is 0.3 m.sup.3/h, the feeding time is 30 min, the reaction temperature is 85° C. and the aging time is 30 min.

(16) In step (4), the slurry viscosity reducer is citric acid with the feeding amount of 8.0 Kg, pH of the slurry F is 6.4, and the discharged water electrical conductivity of washing water is 3.0 ms/cm.

(17) In step (5), the drying method involves drying at an atomization rotation speed in a centrifugal drying tower; the centrifugal drying tower has an inlet temperature of 500° C., an outlet temperature of 140° C. and a pressure of −150 Pa; the rotation speed of the atomizer is 5,500 rpm; and the packaging step is performed by a vacuum packaging machine under a pressure of −200 Pa.

Example 3

(18) A preparation method of high-absorptivity silica as lutein carrier includes (1) adding sodium silicate into a synthesis kettle, introducing steam for heating while stirring, adding water, stirring for reaction to obtain a reaction substrate A, and adding sulfuric acid for pre-acidification until the solution pH is 9.0 to obtain reaction solution B; (2) simultaneously adding sulfuric acid and sodium silicate into the reaction solution B, and performing synthesis reaction to obtain reaction solution C; (3) adding sulfuric acid only into the reaction solution C, for post-acidification until the solution pH reaches 3.8, and aging to obtain dilute slurry D; (4) filtering the dilute slurry D, washing to obtain a filter cake E, transferring to a slurrying machine, and adding a slurry viscosity reducer to obtain slurry F; and (5) drying the slurry F and packaging to obtain silica microspheres as lutein carrier, which is a uniform coarse powder-like silica product.

(19) The sodium silicate in steps (1) and (2) is water solution of sodium silicate with a concentration of 30 Baume, and has a modulus of 3.60.

(20) In step (1), the feeding amount of the sodium silicate is 9.0 m.sup.3, and the concentration of the sodium silicate in the reaction substrate A is 17.0 Baume; the sulfuric acid is water solution of sulfuric acid with a mass fraction of 60%, and the feeding speed and feeding time of the sulfuric acid are 15 m.sup.3/h and 25 min, respectively; the reaction temperature is 50° C.; and the stirring speed is 47 rpm.

(21) In step (2), the sulfuric acid is water solution of sulfuric acid with a mass fraction of 98%, the feeding speed of the sulfuric acid is 0.6 m.sup.3/h, the feeding speed of the sodium silicate is 7.0 m.sup.3/h, the feeding time of the sulfuric acid and the sodium silicate is 55 min, and the reaction temperature is 80° C.

(22) In step (3), the sulfuric acid is water solution of sulfuric acid with a mass fraction of 98%, the feeding speed of the sulfuric acid is 0.3 m.sup.3/h, the feeding time is 35 min, the reaction temperature is 85° C. and the aging time is 20 min.

(23) In step (4), the slurry viscosity reducer is citric acid with the feeding amount of 8.0 Kg, pH of the slurry F is 6.3, and the discharged water electrical conductivity of washing water is 4.0 ms/cm.

(24) In step (5), the drying method involves drying at an atomization rotation speed in a centrifugal drying tower; the centrifugal drying tower has an inlet temperature of 500° C., an outlet temperature of 130° C. and a pressure of −100 Pa; the rotation speed of the atomizer is 7,800 rpm; and the packaging step is performed by a vacuum packaging machine under a pressure of −100 Pa.

Comparative Example 1

(25) A preparation method of high-absorptivity silica as lutein carrier is basically the same as that in Example 1, with the only difference that the modulus of sodium silicate is 2.90.

Comparative Example 2

(26) A preparation method of high-absorptivity silica as lutein carrier is basically the same as that in Example 4, with the only difference that the slurry viscosity reducer is polyacrylic acid.

(27) The performances of high-absorptivity silica as lutein carrier prepared in Examples 1-3 and Comparative Examples 1-2 are tested and the results are shown in the following tables:

(28) TABLE-US-00001 TABLE 1 DBP Bulk Water Absorption Specific Absorption (mL/g) Weight (%) Example 1 3.10 0.21 230 Example 2 2.96 0.225 215 Example 3 3.03 0.215 230 Comparative Example 1 2.85 0.235 205

(29) From Table 1, it can be seen that the high-absorptivity silica as lutein carrier provided by the present invention has high DBP absorption, small bulk specific weight and high water absorption.

(30) TABLE-US-00002 TABLE 2 105° C. 1,000° C. Lutein Heating Loss Loss on Ignition Absorption (%) (%) (%) Example 1 4.7 3.9 250 Example 2 4.4 4.3 235 Example 3 4.6 4.0 245 Comparative Example 2 5.0 4.7 218

(31) From Table 2, it can be seen that the high-absorptivity silica as lutein carrier prepared in Examples 1-3 of the present invention has good stability and higher lutein absorption than that in Comparative Example 2.

(32) TABLE-US-00003 TABLE 3 BET Specific Silica Pore Volume Surface Area Content of Product (m.sup.2/g) (%) (mL/g) Agglomeration Example 1 215 97.8 0.96 No Example 2 240 98.2 1.15 No Example 3 227 97.3 1.06 No

(33) From Table 3, it can be seen that the high-absorptivity silica as lutein carrier provided by Examples 1-3 has large specific surface area and pore volume, high silica content, good dispersibility and no agglomeration.

(34) Those mentioned above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention. In addition, the technical solution of each embodiment can be combined with each other on the basis that those skilled in the art can implement it. When mutual contradiction occurs in the combination of the technical solutions or the combination fails to be implemented, such combination should be considered as inexistent and falling out of the protection scope claimed by the present invention.