Smart Controlled Release of Small Molecules

Lead Research Organisation: University of Birmingham
Department Name: Chemical Engineering

Abstract

There is a growing need to devise methods for stabilisation of active ingredients in liquid and control of their release to the right place at right time, covering a wide range of industrial applications, particularly in the area of small sized molecules. Examples include controlled release of perfumes from fabrics or cosmetic products, delivery of artificial diets to marine fish larvae, bacteriacides in food pipelines, insecticides on soft furnishings or foliage, dyes or inks, adhesives, and drugs in the body. The best way to achieve these objectives is using microcapsules. However, controlling the stability and release of the core chemicals have been proven to be not well understood. In particular, controlling leakage of small molecules is extremely challenging and has not been achieved so far, which has limited the impact and suitability of microcapsules for wide applications. It is proposed to prepare microcapsules having dual shells, which combines the concepts of triggered release (the outer shell may be broken by applied mechanical force) and sustained release (the inner shell with certain permeability). The aim of this project is to formulate and characterise novel double-shell microcapsules with desirable structure and mechanical properties in order to realise stabilisation and controlled delivery of active ingredients made of small molecules, via collaboration between chemical engineering (Professor Z Zhang's group) and chemistry (Professor J Preece and Professor B Vincent, Polymer and Colloid Group in the University Bristol), and between the academic groups and two international companies Appleton Paper Inc., USA, which has three manufacture sites in the UK as a manufacturer of industrial microcapsules and Procter and Gamble, UK (Professor D. York's Technology Breakthrough Group) as an end user of microcapsules.

Publications

10 25 50
 
Description Novel microcapsules with a core of oil-based small molecule hexyl salicylate (a key component of perfume) and shell materials of silica, poly(methylmethacrylate) (PMMA), calcium carbonate, melamine formaldehyde (MF) and PMMA-calcium carbonate composite, silica-calcium carbonate composite, and double shells of MF and calcium carbonate, PMMA and shellac respectively have been prepared using different processing conditions. Their size, shell thickness, mechanical properties and the rate of oil release in aqueous solution have been determined using conventional methods and a new technique. Theoretical analysis has been performed considering the measurable capsule size polydispersity, which allows the estimation of the permeability polydispersity. The new technique is more robust, user friendly and accurate than conventional ones. For a given type of microcapsules, the relationship between processing conditions and their structural and mechanical properties has been established. Microcapsules with a shell of inorganic-organic composite or double shells have shown better performance than those with a single shell in terms of reducing the oil leakage.

A flat membrane of MF made under different processing conditions has also been made, the solubility of the oil in the membrane been measured and the membrane permeability has been determined using standard techniques. It has been found that the membrane permeability strongly depended on the membrane formulation and processing conditions, which has been used to guide preparation of MF microcapsules.

The mechanical property parameters of MF microcapsules with a core of hexyl salicylate, including elastic modulus, elastic limit, yield stress, and the stress-strain relationship to rupture have been determined using micromanipulation compression between two parallel surfaces and finite element analysis (FEA) The microcapsules showed elastic at small deformations, elastic -perfectly plastic at moderate deformations and elastic -perfectly plastic with strain hardening at large deformations leading to rupture. Thus, the complete stress-strain relationship of the shell material has been determined for the first time for core-shell spheres with plastic behaviour. Moreover, the approach has also been applied to mechanical characterisation of silica microcapsules, which ruptured at small deformations near the elastic regime. A general methodology that enables calculation of the rupture stresses leading to the elastic-like rupture of microcapsules under parallel compression testing has been developed. Two scenarios of failure, brittle and ductile, were considered. Analyses of the critical stresses present within the microcapsule shell during different degrees of fractional deformation were obtained using finite element modelling, resulting in similar values for both the brittle and ductile scenarios. Such analysis allows the mechanical strength of microcapsules to be tailored to various controlled release applications via the use of different formulation and processing conditions.

Moreover, MF microcapsules containing perfume oil were prepared using membrane emulsification to generate oil droplets followed by polymerization of MF precondensate on their surface. It has been demonstrated the membrane emulsification resulted in microcapsules with much narrower size and mechanical strength distributions than those made by conventional emulsification based on agitation or homogenisation. Scale-up of the process from lab to pilot-plant scale in collaboration with Leeds University is underway, which if successful can lead to industrial applications.
Exploitation Route The novel, friendly and sustainable microcapsules to be used in consumer products should generate very good publicity of the products. The formulation and processing conditions to prepare novel microcapsules (e.g. PMMA microcapsules) will be exploited to develop more friendly and sustainable microcapsules with better performance than those currently used in commercial detergents.

The understanding of the mechanical strength of microcapsules developed via this project has helped Procter & Gamble commercialise several new detergent products with perfume microcapsules.
Sectors Chemicals,Education,Healthcare,Pharmaceuticals and Medical Biotechnology

 
Description Part of this project involved understanding the mechanical strength of microcapsules, which has helped Procter & Gamble (P&G) develop new detergent products with perfume microcapsules. Recently, Prof. Zhibing Zhang made an entry "Perfume microcapsules in detergents" in association with P&G for the Innovative Product Award of Institution of Chemical Engineers 2014 has been highly commended (http://www.icheme.org/media_centre/news/2014/awards-triumph-for-cyanide-production-technology.aspx#.VF-P3mByZGY).
First Year Of Impact 2012
Sector Chemicals
Impact Types Economic

 
Description Bio-inspired mineralization of alginate hydrogels with hydroxyapatite for new composite materials in tissue engineering 
Organisation Norwegian University of Science and Technology (NTNU)
Country Norway 
Sector Academic/University 
PI Contribution This is a confernece paper resulting from collaboration with Dr Pawel Sikorski's group, Department of Physics, Norwegian University of Science and Technology
Start Year 2010
 
Description Evaluation of microcapsule wall strength 
Organisation University of Sheffield
Country United Kingdom 
Sector Academic/University 
PI Contribution Collaboration with Professor Steve Armes' group, Department of Chemistry, University of Sheffield, UK
Start Year 2009
 
Description Media interest 
Form Of Engagement Activity A press release, press conference or response to a media enquiry/interview
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Professional Practitioners
Results and Impact Dissemination / Communication has been made mainly via publishing journal papers, attending international and national conferences, visits to companies and other academic institutions.

Prof. Zhibing Zhang's entry on "Perfume microcapsules in detergents" in association with Procter & Gamble for the Innovative Product Award of Institution of Chemical Engineers 2014 has been highly commended (http://www.icheme.org/media_centre/news/2014/awards-triumph-for-cyanide-production-technology.aspx#.VF-P3mByZGY).
Year(s) Of Engagement Activity 2014
URL http://www.youtube.com/watch?v=SltXHwGDMqA