1.1 Research and development trends
Microencapsulation is a knowledge-intensive and dynamic research field with an increasing growth of publications. Trends in patent vs. non-patent literature on microencapsulation illustrate the growth of basic research (scientific articles), as well as the fast growth of industrial research, represented in waves of patented inventions (Figure 1).
Among numerous possible applications fields, microencapsulation offers many opportunities to improve the properties of textiles or to give them new functions.
A bibliometric analysis of scientific articles in the Web of Science , and patents in the Espacenet database  reveals that the first ideas of applying microcapsules in textiles emerged in the early 1970s, and that the majority of publications on microencapsulation for textile applications remain patents (Figure 2). This emphasises the importance of industrial property rights, and the strong participation of industrial research in the development of added-value functional textiles, invented with microencapsulated active ingredients.
2 Microencapsulation methods and processes of applying microcapsules to textiles
2.1 Microencapsulation methods
The selection of microencapsulation process for added-value textile applications depends on the desired characteristics and uses of the products. For example, microcapsule size, shape, wall material, active substance, release mechanism, method of application, and compatibility with other components of the formulation must be adapted to the requirements of textile processing methods, and uses of the final product.
Most often, microcapsules for textile applications have been prepared by one of the following technological possibilities:
Coacervation processes (e.g. gelatin-gum arabic microcapsule walls) taking place in colloid systems, where macromolecular colloid rich coacervate droplets surround dispersed microcapsule cores, and form a viscous microcapsule wall, which is solidified with crosslinking agents (Figure 3).
Polymerization methods, where monomers polymerize around droplets of an emulsion and form a solid polymeric wall. In in situ polymerization (e.g. aminoaldehyde resin walls), monomers or precondensates are added only to the aqueous phase of emulsion (Figure 4), while in interfacial polymerization (e.g. polyamide, polyester, polyurethane walls), one of the monomers is dissolved in the aqueous phase and the other in a lipophylic solvent.
Physical/mechanical methods (e.g. spray-drying, fluidized bed coating, extrusion, deposition in vacuum, solvent evaporation from emulsions, ultrasonic liposome formation), where the microcapsule wall is mechanically applied, condensed or layered around the microcapsule core. Physical/mechanical microencapsulation methods are used to design microcapsules that release their content during textile dyeing, washing or drying; the walls are soluble or heat sensitive to dissolve or melt at a desired circumstance.
In situ polymerization is one of the chemical microencapsulation processes often used for technical applications, including textiles. The process takes place in oil-in-water emulsions; the result is nicely smooth, spherical, reservoir-type microcapsules with transparent polymeric pressure-sensitive microcapsule walls (Figures 5 and 6). Typical wall materials for in situ polymerization are aminoplast resins, such as melamine–formaldehyde, urea-formaldehyde, urea–melamine-formaldehyde or resorcinol-modified melamine–formaldehyde polymers. The in situ processes (Figure 7) can start either directly from amine and aldehyde monomers, or from the precondensates. Typically, all materials for the formation of microcapsule wall originate from the continuous aqueous phase of the oil-in-water emulsion system, and therefore have to be water-soluble. To achieve better process control and improved mechanical properties of microcapsules, modifying agents/protective colloids are added, such as styrene-maleic acid anhydride copolymers, polyacrylic acid, or acrylamidopropylsulfonate and methacrylic acid/acrylic acid copolymers .
For some technical applications the in situ aminoaldehyde microcapsules remain irreplaceable, due to some superior characteristics, such as:
the spherical reservoir-type shape with thin impermeable transparent walls (Figure 8);
high chemical and thermal stability;
high microcapsule resistance to harsh chemical environments (e.g. in detergents, softeners etc.);
good storage stability;
high microencapsulation yields (≥ 99%);
effective microencapsulation process control;
controllable microcapsule size and size distribution;
good transferability of the in situ process to large-scale industrial production.
In addition, wall permeability and mechanical characteristics can be regulated and adapted, to obtain tailor-made pressure-sensitive or more elastic microcapsules with controled diffusion, to support different release mechanisms of the products [3, 4]. The main constraint of the in situ process is synthetic nature of aminoaldehyde microcapsule wall, and the residual formaldehyde in microcapsule suspension after the polycondensation process, which limits the in situ microcapsules to technical products. However, with the optimised selection of process parameters and application of formaldehyde scavengers, the concentration of free formaldehyde can be minimized to meet the technical standards for textiles [5–9].
2.2 Processes of applying microcapsules to textiles
Microcapsules have to be formulated for applications on woven or nonwoven textiles without substantially altering the feel or color of textile products. Formulation additives usually consist of binders, crosslinking agents, organic or inorganic pigments and fillers, antifoaming agents and/or other surfactants, and viscosity-controling agents/thickeners.
Binders play a crucial role in microcapsule formulations for textiles. To a large extent, they determine the quality, durability and washability of textile materials with microencapsulated ingredients. Typically, binders are selected from the groups of:
water-soluble polymers, such as polyvinyl alcohol, carboxymethyl cellulose, starch and modified starches, xanthanes, alginates, and other natural gums;
synthetic latexes, such as polyacrylate latexes, styrene-butadiene, polyvinyl-acetate, ethylene–vinyl acetate copolymers;
synthetic resins, such as such as urea–and melamine–formaldehyde resins, dimethylol ethylene urea, dimethylol dihydroxy ethylene urea, dimethylol propylene urea, polyurethane and epoxy resins, vinyl acetate resins;
synthetic rubbers, such as polyurethanes, nitrile and chloroprene rubbers;
Different techniques can be used for applications of microcapsules to textiles. Patents describe incorporation of microencapsulated compounds onto or into textiles by:
coating with an air knife or rod coater;
impregnation or immersion (Figure 9);
printing techniques, such as screen-, photographic-, electrostatic-, pressure-transfer, thermal transfer and inkjet printing;
spraying on the surface of textiles;
inclusion of microcapsules into the textile fibers during the spinning process, such as polyester, nylon or modacryl fiber material;
incorporation into polymer foams, coatings and multilayer composites that are placed or inserted into selected parts of textile clothing or footwear.
3 Purposes and release mechanisms of microcapsules in textile products
Mechanisms of releasing active ingredients from the microcapsule cores depend on the purpose of microencapsulation, on functions and desired effects of encapsulated components, and on the microcapsule wall characteristics, particularly on permeability. An overview of microencapsulation purposes and release mechanism in textile products is given below, with examples of patented inventions presented in Chapter 4.
In textile applications, microcapsules with permeable walls enable:
Prolonged/sustained release of active components from the core. This principle is used in long-lasting perfumes and deodorants on textile carriers, in insect repellent textiles, and in sustained release cosmetic and medical textiles.
Separation of low and high molecular weight molecules can be applied in microencapsulated enzymes in detergent compositions for machine washing of textiles.
Microcapsules with impermeable walls are used in formulations and products where temporary isolation and quick release of active components are necessary. Examples of useful functions and effects, achieved by applying impermeable microcapsules to textiles, include the following:
Protection of substances against environmental effects: microcapsule walls protect unstable components against environmental influences, and release them only under the desired circumstances. For instance, microencapsulated vitamins, lipids and essential oils in cosmetic textiles are protected against oxidation; microencapsulated enzymes and oxidants are stabilized when added to laundry formulations for textiles.
Separation of reactive components: this is used when leuco dyes are separated from color developers in thermochromic textiles, or to separate reactants in formulations of multicomponent adhesives and binders for textile bonding.
Locally limited activity is applied to enable special color effects, such as reversible color changes, speckled patterns and glossy effects, or to reduce the migration of dyes in multicolor textile printing.
Reduction/prevention of volatility: this ensures that volatile compounds, such as perfumes, fragrances and antimicrobial essential oils are retained in fragranced textiles until they are released in a target situation.
Conversion from a liquid into a solid state: this is beneficial in formulations of powdered adhesives with microencapsulated solvents for textile-containing laminate bonding; liquid crystals are encapsulated and used in color changing textiles.
To release microencapsulated active components from microcapsule cores, numerous ways of release mechanisms have been invented and applied in added-value textile products (Figure 10), such as:
The mechanism of external pressure, which breaks the microcapsule wall and releases the core, was the first developed and is still widely used, for instance in antimicrobial agents for socks and textile shoe inserts (mechanical pressure caused by walking), fragranced textiles, such as t-shirts, ties, handkerchiefs, pillows and linen (release by pressure and rubbing), and pressure-sensitive multicomponent adhesives for textile bonding (activation in a mechanical press).
In some applications, microcapsule wall breaks because of inner pressure. This happens if the core contains substances which, under special conditions (e.g. UV light), decompose into gaseous components. The effect is used in blowing agents in the production of light synthetic leather.
The core substance can be released by abrasion of the microcapsule wall, e.g. in antistatics and fragrances in textile washing and drying.
In many applications, core materials are released by heat that causes melting of microcapsule wall at a specifically designed temperature. Examples include components in cosmetic and medical textiles (release at body temperature), and textile softeners and fragrances in formulations for dryers (release by heat).
Microencapsulated fire retardants or extinguishers, released by burning, are used in fire-proof textile materials for carpets, curtains, fire-protecting clothes, and car interiors.
Microcapsules in photographic and light-sensitive textile printing processes are decomposed or hardened by light.
In textile washing/cleaning compositions, microcapsules with active ingredients dissolve in a specific solvent (most often water), sometimes only at a selected pH value of the washing cycle.
In textile processing formulations, selected reagents may be released by enzymatic degradation of target microcapsules.
In specific applications, permanent enclosure of the core material within the resistant microcapsules is essential. Examples include microencapsulated phase change materials (PCMs) for active thermal control, where microcapsules hold the PCM solid-liquid transitions, and for liquid crystals in reversible color changing textiles.
4 Applications of microcapsules in textile products
The possibilities for using microencapsulation technologies in textile products are numerous, and include coloring materials, enzymes, fire retardants, adhesives, fragrances, perfumes, insect repellents, disinfectants, cosmetic additives, decontaminants, PCMs, UV absorbers and self-healing agents (see Figure 11).
4.1 Microencapsulated dyes and pigments for textile dyeing and printing
Microencapsulation of dyes and pigments for dyeing and printing is one of the oldest microencapsulation applications in textile processing. The idea of including microencapsulated dyes and pigments found their place in different techniques, such as dyeing and printing by electrostatic fields, solvent dyeing, dot dyeing and multicolored speckled printing, pressure or thermal transfer printing, screen printing, photographic screen printing, and ink jet textile printing (Table 1).
4.2 Textiles with microencapsulated thermochromic materials
Thermochromism, the reversible dependence of color on temperature, utilizes temperature change to initiate color development or color fading. Thermochromic systems can involve inorganic compounds, such as transition metal and organometallic systems, or organic compounds, including liquid crystals, stereoisomerism and molecular rearrangement. Thermochromic systems based on liquid crystals and molecular rearrangement have been applied successfully in textiles on a commercial scale . Examples are presented in Table 2.
4.3 Textiles with microencapsulated photochromic materials
Photochromic dyes absorb quanta in the visible or near-infrared light region. The excited state of a dye must last long enough to undergo a chemical reaction. Applications of photochromic dyes are known for invisible writing, erasable recording media, darkening of sunglasses, or darkening of textile products, such as curtains, t-shirts and sportswear . Microencapsulation of photochromic dyes for textile applications is presented in Table 3.
4.4 Microencapsulated catalysts and enzymes for special textile effects
4.5 Textiles with microencapsulated fire retardants
One of the shortcomings of untreated textile materials used for decoration and construction purposes is their flammability. As a solution, flame retardant textiles have been developed with incorporated fire retardants. A review of microencapsulation of flame retardant formulations suitable for application in textiles was published by Salaün et al. . Microencapsulation can be used to avoid reactions of fire retardants with textile polymers, prevent sublimation or exudation of fire retardants from the polymer, or to eliminate substance hydrophilicity. The idea of microencapsulated fire retardants for textiles was first launched by the industrial producers in the beginning of the 1970s. Textiles treated with microencapsulated fire retardants have been used for military and civilian clothing and tents, for carpets, furniture and car interiors (Table 5).
4.6 Microencapsulated agents for textile sizing and adhesive bonding
4.7 Microencapsulated blowing agents and expandable microcapsules for leather substitutes
4.8 Microencapsulation for textile water proofing
Increased impermeability and water proofing of textile surfaces can be achieved by expanding a layer of microcapsules on a porous support into an impermeable layer, or by applying microencapsulated water proofing agents, and releasing them from microcapsule cores. In both cases, heat treatment plays a crucial role in microcapsule activation (Table 8).
4.9 Microcapsules in textile softening and antistatic compositions
Fabric softeners and antistatics for textile washing and drying employ microcapsules to solve the incompatibility of antistatic compounds and anionic surfactants in detergents, to incorporate liquid ingredients into solid formulations, to add hydrophobic components into water-based formulations, and to achieve a prolonged release of fragrances (Table 9).
4.10 Microencapsulated ingredients in textile detergents
There are patents on microencapsulated components in detergent formulations for washing textile goods. The main applications include microencapsulated enzymes (Table 10); bleaching and whitening agents (Table 11); and perfumes and other additives, such as dry defoamers, dyes and cleaning chemicals (Tables 12 and 13).
In early patents, enzyme encapsulation improved detergent storage stability, reduced dusting and minimized health hazards in detergent factories and households. Subsequently microencapsulation was used to protect enzymes against the activity of aggressive additives, especially bleaches. Newer patents used the advantage of encapsulation to incorporate enzymes into liquid and gelled detergent formulations (Table 10).
4.10.2 Bleaching agents and whiteners
Microencapsulated bleaching agents in laundry formulations have the advantages of being separated from the oxidation sensitive components in the detergent compositions, to prevent reduction of their bleaching capacity, and to reduce the damage to fabrics (Table 11).
4.11 Textiles with microencapsulated fragrances and perfumes
Fragranced textiles, containing microencapsulated essential oils, aromas and perfumes, have been developed to either slowly release their contents through permeable walls, or to have completely impermeable walls, and open only by application of mechanical pressure and rubbing whenever the wearer moves. A combination of both release mechanisms is also possible. After the problems of controling the release have been solved, and better washfast binders introduced, a new generation of aromatic textiles entered the market that remain fragrant over a prolonged period of time, resist dry cleaning, or keep the microcapsules over several washing cycles. Applications of microencapsulated fragrances, perfumes and antimicrobial essential oils in woven and nonwoven textiles range from perfumed curtains, bed linen, shirts, socks and hosiery to antimicrobial towels, shoe insoles, and textiles for seats in public transportation (Table 14). Figures 12–15 illustrate some examples of our own research .
4.12 Textiles with microencapsulated animal repellents
To obtain prolonged insecticidal and insect repellent effects of fibers and textiles, and to reduce the toxicity and volatility of active compounds, insect repellents and/or insecticides can be microencapsulated and applied to textiles (Table 15).
In addition to insect repellents, other animal repellents have been microencapsulated. For instance, prolonged release microencapsulated deer and rabbit repellents on nonwoven textiles were developed for horticultural and agricultural use .
4.13 Textiles with microencapsulated antimicrobial, disinfectant and deodorant components
Several essential oils and plant extracts have antimicrobial and deodorant properties. Because they are liquids, microencapsulation is required for the conversion into the solid state. At the same time, a prolonged activity of microencapsulated active substances can be achieved.
Inventions on microencapsulated antimicrobials for textile applications include various textile coating compositions with antimicrobial effects, as well as specific coating procedures and additives (Table 16).
As an example of our work, we developed antimicrobial textile shoe insoles, based on nonwoven polyester textiles, impregnated with a mixture of microencapsulated essential oils of sage, lavender and rosemary (Figure 16). Pressure-sensitive aminoaldehyde resin microcapsules with partially permeable walls were prepared using a modified in situ polymerization method. For the impregnation of textiles, a technique for the transport of the textile carrier through the impregnation basin was used. Product testing proved the sustained release of essential oils from microcapsules in worn shoe insoles, and antimicrobial activity of the essential oil mixture against the microorganisms Staphylococcus aureus, Candida albicans and Trichophyton mentagrophytes [142, 143].
4.14 Bioactive medical and cosmetic textiles with microencapsulated ingredients
In the 1990, the first inventions of medical and cosmetic textiles introduced added-value textile products with prolonged effects, such as antimicrobial effects, accelerating blood circulation, improving the physiological condition of skin, skin hydration, ageing prevention, or skin whitening. Soon other inventions followed, aiming at pain relief, itch suppression, accelerating the metabolism of water, reducing cellulite, and similar effects. The microcapsules are typically not broken when produced, processed, or laundered, but gradually burst open when the textiles are worn. The formulations are applied to the fabrics by soaking, coating or spraying; microcapsules can also be formulated as sprays, which tightly adhere the microcapsules to textile structures, such as hosiery, underwear, bedlinen, and bandages (Table 17).
4.15 Textile decontaminants, filters and odor absorbers
4.16 Textiles for active thermal control
Textiles for active thermal control have been one of the fast growing product areas of microencapsulation technology applications (Table 19). In addition to attempts to convert sunlight energy into chemical and later thermal energy, a wave of inventions and practical applications utilized microencapsulated PCMs that absorb or emit heat at their phase change transition temperature (Figure 17). Typical examples of PCMs are strait chain paraffinic hydrocarbons with 13 to 28 carbon atoms, and the phase change temperatures ranging from −5.5 °C to +61 °C. As they are flammable and liquid above the phase transition temperature, microencapsulation is essential for their practical use in various thermal management applications. In functional textiles, microencapsulated PCMs function as heat absorbers or as barriers against cold, and are incorporated into products with enhanced thermal properties and active thermal control .
The choice of suitable PCMs depends on the latent heat of the phase change and the transition temperature. In general, the higher the PCM’s latent heat of phase change, the more thermal energy a material can store. According to their phase change temperature ranges, the PCMs are categorized into three main groups – the heating, the cooling and the buffering PCMs :
The phase transition temperature of the heating PCMs is above the body’s normal skin temperature. When a heating PCM is warmed above its transition temperature and placed in thermal contact with the skin, the temperature gradient flows from the PCM into the body.
The cooling PCMs have a phase transition temperature below the body’s normal skin temperature. When chilled below their transition temperature, the temperature gradient flows from the body into the PCM.
The phase transition temperature of the buffering PCMs is slightly below the normal body temperature. These materials absorb or release heat depending on environmental and metabolic conditions.
To include PCM microcapsules into textile products, different systems have been developed, such as:
the incorporation of PCM microcapsules into the textile fibers before or during the spinning process;
the coating of fibers and fabrics with compositions of PCM microcapsules and binders;
the insertion of polymer foams with microcapsules PCM into textile products;
the preparation of complex composites with three or more layers.
4.17 Microcapsules in self-cleaning textiles and self-healing fibers
5 Concluding remarks
The idea of using microencapsulation technology in added-value textile products was born soon after the introduction of the large-scale production of microcapsules for pressure-sensitive copying papers. Microencapsulation for textiles became a research and development area with a strong industrial intellectual property protection, as patent documents outnumbered scientific articles. In the past some reviews were prepared to summarize research and development achievements [111, 174–178]. The survey in this chapter, prepared by analysis of inventions from the beginning of the microencapsulation technology to the present day, reveals that the first burst of patents on microcapsules for textiles in the 1970s brought the following microencapsulated products: (i) dyes and pigments for special textile dyeing and printing techniques; (ii) catalysts, crosslinking agents and enzymes for textile treatment; (iii) reagents for textile sizing and bonding; (iv) fire retardants for fire-resistant textiles; (v) expandable microcapsules for the production of light weight leather substitutes and water proofing of porous textile surfaces; (vi) fragrant textiles with microencapsulated essential oils and aromas; (vii) ingredients in textile detergents and softeners, including enzymes, bleaches, softeners and antistatics for textile washing and drying compositions.
After a short stagnation of research in the beginning of the 1980s, there was a second wave of textile microcapsule patents, with new concepts of the following microecnapsulated products: (viii) thermochromic materials, which utilized temperature changes for color development and fading, and microencapsulated photochromic dyes – the results being thermochromic sports and leisure garments, and photochromic curtains, sportswear and shirts; (ix) blowing agents and expandable microcapsules for leather substitutes and textile water proofing; (x) components in textile filters, odor absorbers and decontaminants.
After 1990, the inventions were further extended and upgraded to: (xi) prolonged release bioactive medical and cosmetic textiles with microencapsulated bioactive/healing components; (xii) antimicrobial, disinfectant and deodorant textiles; (xiii) repellent and insecticidal textiles, (xiv) functional textiles with heat storing and releasing properties, based on microencapsulated PCMs, applied in sportswear and special technical apparel with active thermal control.
After the year 2000, new inventions appeared in almost all previously known application fields, particularly in the domains of microencapsulated thermochromic and photoschromic dyes for color changing fabrics and sensor fibers; new techniques and solutions in textile dyeing and printing, involving microcapsules; and microencapsulation of additives in sophisticated compositions of textile detergents and softeners.
Since 2010 a new generation of microcapsule-based inventions have been emerging, applying microencapsulated components to achieve (xv) self-cleaning and/or self-healing properties of high-tech smart textiles.
The research on microencapsulation was financially co-supported by: the Faculty of Natural Sciences and Engineering, University of Ljubljana; the Slovenian Research Agency (projects L2-5571, L1-6230 and L4-1562); and by the ERO, Chemical, Graphic and Paper Manufacturers, d.d. Celje, Slovenia. Samples of textiles with microcapsules for SEM imaging were kindly provided by Boštjan Šumiga, Ph.D., and Mr. Emil Knez from the AERO company.
This article is also available in: Giamberini (et al.), Microencapsulation. De Gruyter (2015), isbn 978-3-11-033187.
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