Pickering emulsion stabilized by cellulose nanocrystals from ginkgo seed shells and preparation method thereof

Patent metadata

Field	Value
Publication number	US-12115221-B2
Application number	US-202117216771-A
Country	US
Kind code	B2
Filing date	Mar 30, 2021
Priority date	Oct 31, 2019
Publication date	Oct 15, 2024
Grant date	Oct 15, 2024

Abstract

The disclosure discloses a Pickering emulsion stabilized by cellulose from ginkgo seed shells and a preparation method thereof, and belongs to the fields of preparation methods of biomass materials and food chemical industry. The disclosure uses ginkgo seed shells as a raw material to obtain high-purity cellulose through hot alkali treatment and sodium chlorite bleaching. After the cellulose is dried, the cellulose is hydrolyzed with sulfuric acid to obtain a cellulose nanocrystal suspension. The suspension is mixed with an oil phase, and the Pickering emulsion is obtained through high-speed shearing and homogeneous emulsification. The disclosure can prepare cellulose nanocrystals with different aspect ratios by adjusting the parameters of high-speed shearing and homogeneous emulsification according to actual production needs. Cellulose nanocrystals with high aspect ratio can be used to prepare stable Pickering emulsions with high oil phase and high viscosity, which can be applied to the fields of food, cosmetics and the like; and cellulose nanocrystals with low aspect ratio can be used to prepare Pickering emulsions with low viscosity and high fluidity, which can to be applied to the fields of food and medicine.

First claim

What is claimed is:

1. A method for preparing a Pickering emulsion using cellulose from ginkgo seed shells, comprising the following steps:
(1) purifying cellulose from ginkgo seed shells: mixing crushed ginkgo seed shells with a preheated 2-5 wt % sodium hydroxide solution in a material-liquid ratio of 1:20 to 1:40 (w/v); then heating the mixture in a water bath at 80-100° C. for 1-3 h; carrying out filtering and washing with deionized water 2-4 times; then carrying out drying with hot air at 40-60° C. to obtain a dried cellulose; mixing the dried cellulose with a rinsing solution in a material-liquid ratio of 1:20 to 1:50 (w/v); heating the mixture in a water bath at 80-100° C. for 1-3 h; then filtering the mixture to remove the rinsing solution; and carrying out drying with hot air at 40-60° C. to obtain dried cellulose powder;
(2) preparing cellulose nanocrystals (CNCs): mixing the dried cellulose powder obtained in step (1) with a preheated sulfuric acid solution with a mass concentration of 58-64% for carrying out a hydrolysis reaction, wherein a hydrolysis temperature is 40-50° C., the hydrolysis reaction time is 10-60 min, and a material-liquid ratio of the cellulose to the sulfuric acid solution is 1:10 to 1:20 (w/v); after the hydrolysis, immediately terminating the hydrolysis reaction with 10-15 times of deionized water by volume; then carrying out centrifugation to remove a sulfuric acid hydrolysate; redispersing centrifuged precipitate into deionized water to obtain a suspension; filling a dialysis bag with the suspension; and repeating dialysis with deionized water until a pH value of the suspension is stable to obtain a cellulose microcrystal suspension;
(3) preparing cellulose nanocrystals with different aspect ratios: homogenizing the cellulose suspension obtained in step (2), wherein a homogenization pressure is 10-100 MPa, the number of cycles is 4, and a homogenization temperature is room temperature; cellulose nanocrystals with high aspect ratios are obtained by homogenization treatment at a pressure of 10-30 MPa; and cellulose nanocrystals with low aspect ratios are obtained by homogenization treatment at a pressure of 30-100 MPa; and
(4) preparing the Pickering emulsion: mixing the cellulose nanocrystals in step (3) used as a solid particle emulsifier with an oil phase, and carrying out emulsification to obtain the Pickering emulsion.

2. The method of claim 1 , wherein in step (4), the cellulose nanocrystals with high aspect ratios are mixed with 50%-80% of an oil phase, and emulsification is carried out to obtain a Pickering emulsion with a high oil phase and high viscosity; or the cellulose nanocrystals with low aspect ratios are mixed with 10%-50% of an oil phase, and emulsification is carried out to obtain a Pickering emulsion with low viscosity and high fluidity.

3. The Pickering emulsion prepared by the method of claim 1 , wherein the Pickering emulsion is stabilized by cellulose from ginkgo seed shells.

4. The Pickering emulsion prepared by the method of claim 2 , wherein the Pickering emulsion is stabilized by cellulose from ginkgo seed shells.

5. A method of preparing a Pickering emulsion, comprising the following steps:
(1) treating crushed ginkgo seed shells with a hot alkali solution, then carrying out rinsing with a rinsing solution, and carrying out drying with hot air to obtain high-purity cellulose from ginkgo seed shells;
(2) hydrolyzing the cellulose from ginkgo seed shells obtained in step (1) with sulfuric acid; after the hydrolysis, adding deionized water immediately to terminate a hydrolysis reaction; centrifuging a hydrolysate to obtain a precipitate; dialyzing the precipitate with deionized water to remove inorganic salt ions; and obtaining a cellulose microcrystal suspension after dialysis;
(3) homogenizing the cellulose suspension obtained in step (2), and preparing cellulose nanocrystals (CNCs) with different aspect ratios by adjusting a homogenization pressure; and
(4) using the cellulose nanocrystals in step (3) as a solid particle emulsifier, diluting the cellulose nanocrystals with deionized water to serve as a water phase, mixing the water phase with an oil phase, and carrying out emulsification to obtain the Pickering emulsion.

6. The method of claim 5 , wherein the rinsing solution in step (1) contains 1.5-2.0 g of sodium chlorite, 2.5-3.0 g of sodium hydroxide and 7-8 mL of glacial acetic acid for each 100 mL.

7. The method of claim 5 , wherein in step (2), a mass concentration of the sulfuric acid solution used for sulfuric acid washing is 58-64%, a hydrolysis temperature is 40-50° C., the hydrolysis reaction time is 10-60 min, and a material-liquid ratio of the cellulose to the sulfuric acid solution is 1:10 to 1:20 (w/v).

8. The method of claim 5 , wherein conditions for preparing the cellulose nanocrystals with different aspect ratios in step (3) are as follows: a homogenization pressure is 10-100 MPa, the number of cycles is 4, and a homogenization temperature is 25° C.; CNCs with high aspect ratios are obtained by homogenization treatment under a pressure of 10-30 MPa; and CNCs with low aspect ratios are obtained by homogenization treatment under a pressure of 30-100 MPa.

9. The method of claim 5 , wherein in step (4), a concentration of the cellulose nanocrystals in the water phase is 0.10-0.50 wt %.

10. The method of claim 5 , wherein the oil phase in step (4) comprises corn oil, soybean oil and peanut oil.

11. The method of claim 5 , wherein the emulsification in step (4) is carried out by adopting a high-speed shearing process or a homogenization process or a combination of the two processes to prepare the Pickering emulsion, wherein conditions for the high-speed shearing process are as follows: a shearing rate is 8000-10000 rpm, and the shearing time is 1-3 min; and conditions for the high-pressure homogenization process are as follows: a homogenization pressure is 10-30 MPa, and the number of cycles is 2-4.

12. The Pickering emulsion prepared by the method of claim 5 , wherein the Pickering emulsion is stabilized by cellulose from ginkgo seed shells.

13. The Pickering emulsion prepared by the method of claim 6 , wherein the Pickering emulsion is stabilized by cellulose from ginkgo seed shells.

14. The Pickering emulsion prepared by the method of claim 7 , wherein the Pickering emulsion is stabilized by cellulose from ginkgo seed shells.

15. The Pickering emulsion prepared by the method of claim 8 , wherein the Pickering emulsion is stabilized by cellulose from ginkgo seed shells.

16. The Pickering emulsion prepared by the method of claim 9 , wherein the Pickering emulsion is stabilized by cellulose from ginkgo seed shells.

17. The Pickering emulsion prepared by the method of claim 10 , wherein the Pickering emulsion is stabilized by cellulose from ginkgo seed shells.

18. The Pickering emulsion prepared by the method of claim 11 , wherein the Pickering emulsion is stabilized by cellulose from ginkgo seed shells.

Assignees

• Univ Jiangnan
• Jiangnam Univ

Inventors

• Fan Liuping
• Ni Yang
• Li Jinwei

Classifications

• C09K23/56

  Glucosides; Mucilage; Saponins · CPC title

• C09K23/00

  Use of substances as emulsifying, wetting, dispersing, or foam-producing agents · CPC title

• C08B15/08

  Fractionation of cellulose, e.g. separation of cellulose crystallites · CPC title

• C08B1/003

  Preparation of cellulose solutions, i.e. dopes, with different possible solvents, e.g. ionic liquids (solutions used in the manufacture of monocomponent artificial filaments or cellulose or derivatives thereof D01F2/02) · CPC title

• A61K9/1075

  Microemulsions or submicron emulsions; Preconcentrates or solids thereof; Micelles, e.g. made of phospholipids or block copolymers (A61K9/0026 takes precedence) · CPC title