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Silica microcapsules and methods of preparing same

A silicon dioxide and microcapsule technology, applied in the directions of microcapsule preparation, microsphere preparation, capsule delivery, etc., can solve problems such as prolonged consumption time

Active Publication Date: 2018-12-21
INTERNATIONAL FLAVORS & FRAGRANCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Challenges remain in large-scale manufacturing following this method, such as the prolonged time spent in isolation and the use of large quantities of expensive pure silica precursors

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0119] The silica microcapsules of the present invention, Microcapsule 1, were prepared according to the following procedure.

[0120] 40 g of tetraethylorthosilicate (TEOS) (commercially available from Evonik Corporation, Piscataway, NJ) was added to 36 g of 0.01N hydrochloric acid, and the mixture was stirred at 45°C for 30 minutes. An additional 376 g of TEOS was added dropwise over 1 hour. The mixture was stirred at 45°C for 16 hours and loaded into a Rotavapor to remove lights with the aid of a 10 mmHg vacuum. The resulting 275 g colorless liquid polysiloxane material (Poly-Si) was saved and used for capsule preparation. The polysiloxane material thus prepared has a viscosity of 5-30 (Brookfield DV1 viscometer, 60 rpm, ambient temperature, spindle 4), and a molecular weight of 1000-3000.

[0121] A solution of 2 g of Gelatin A (commercially available from Great Lakes Gelatin Co., Grayslake, IL) in 118 g of water was heated to 50°C. In 10 g of pretreated silica polysili...

Embodiment 3

[0131] The third microcapsule of the present invention, microcapsule 3, was prepared according to the procedure described below.

[0132] Step 1: Preparation of fragrance silica microcapsules using sorbitan ester

[0133]By mixing 1 g of Span 80 (sorbitan monooleate, commercially available from Sigma-Aldrich) and 9 g of Tween 80 (polyoxyethylene sorbitan monooleate, commercially available from Sigma-Aldrich) Mix in 300 g of water with stirring for 2 hours to prepare a surfactant solution. 100 g of this surfactant solution was added to the oil phase containing 10 g of pretreated silica polysilicon, 25 g of fragrance accord and 5 g of Neobee oil. The resulting mixture was homogenized with an Ultra Turrax homogenizer at 9000 rpm for 3 minutes. The homogenizer was replaced with an overhead stirrer and the slurry was stirred at 400 rpm and the pH was adjusted to 8.5 with dilute ammonia solution. The mixture was stirred at room temperature for 16 hours to obtain a capsule slurry ...

Embodiment 4

[0139] Another microcapsule of the present invention, microcapsule 4, was prepared according to the following procedure.

[0140] A sol-gel mixture was prepared by adding 30 g of pretreated silica polysilicon and 40 g of lemon flavor oil (commercially available from International Flavors & Fragrances, South Brunswick, NJ). To this sol-gel mixture was added 180 g of a 10% aqueous solution of superpure gum. The resulting mixture was homogenized with an Ultra Turrax homogenizer at 10000 rpm for 2 minutes to obtain a microcapsule slurry. Chitosan (3.6 g in 360 g of a 1% aqueous solution) was added. The resulting microcapsule slurry was stirred at room temperature for 24 hours to obtain Microcapsule 4.

[0141] Extractable oil analysis indicated 84.5% EE. The microscope image of microcapsule 4 showed that it was stable for at least 2 days after drying at room temperature on a microscope slide.

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Abstract

Disclosed is a microcapsule containing: (i) a microcapsule core having an active material, and (ii) a microcapsule wall formed of a first polymer and second polymer. The first polymer is a sol-gel polymer. The second polymer is gum arabic, purity gum ultra, gelatin, chitosan, xanthan gum, plant gum, carboxymethyl cellulose, sodium carboxymethyl guar gum, or a combination thereof. The weight ratiobetween the first and second polymer is 1:10 to 10:1. Also disclosed are processes for preparing the microcapsule and uses of the microcapsules in consumer products.

Description

Background technique [0001] Microcapsules are used for the controlled release of flavors, fragrances and nutrients. They also protect sensitive food ingredients from breakdown. Despite the progress in microencapsulation technology, developing food-grade microcapsules remains a challenge due to limited materials suitable for food consumption. [0002] Sol-gel microcapsules such as silica microcapsules have been used to deliver fragrances for personal care products such as antiperspirant products. See US Patent No. 9,044,732 and US Patent Application Publication Nos. 2012 / 0104639 and 2004 / 0256748. These microcapsules contain silica microcapsule walls usually prepared in the presence of cetyltrimethylammonium chloride (CTAC). Dioxide, as a naturally abundant material, has been recognized by the Food and Drug Administration and other health organizations such as the World Health Organization and the European Food Safety Authority Safe food additive. However, CTAC is a non-foo...

Claims

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Application Information

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IPC IPC(8): B01J13/02A23L27/00A61L9/01C08L5/00C08L83/14
CPCA61L9/01C08L5/00A23L27/00A61L9/012A61L9/048B01J13/10B01J13/14B01J13/206B01J13/22C08L1/286C08L5/08C08L89/06A23P10/30A23L27/72A23L27/74C08L83/04A23P10/35A21D2/02A21D2/165A23G4/064A23V2002/00A61K8/11A61K9/4816A61K9/4825B01J13/08A23F3/12A23F3/14A23F3/18
Inventor 约翰·布拉姆斯罗纳德·加巴德耿峰朱莉·安·维伦兰德徐力刘易斯·迈克尔·波普尔韦尔
Owner INTERNATIONAL FLAVORS & FRAGRANCES
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