Optimisation of solvolysis for recycling carbon fibre reinforced composites

Solvolysis processes have been used to degrade the resin of two different varieties of epoxy based carbon fibre reinforced composite (CFRC) materials. A degradation of up to 98% has been achieved when processing material at a temperature of 320 °C using a supercritical solvent mixture of acetone and water. Increasing the processing time from 1 to 2 hours shows an increase in the degradation of only 10% and there does not appear to be any benefit in processing the material beyond this time. Due to the batch conditions used, it is necessary to rinse the fibres with acetone after processing to remove remaining organic residue. Washing the fibres at supercritical batch conditions, however, does not efficiently remove the residue compared to a simple hand washing with acetone. Shredding the sample prior to processing also does not have a significant effect. The process investigated requires 19 MJ.kg-1 of fibres recovered and, since the process has not yet been optimised, shows strong potential for future development especially since it allows for the recovery and reuse of organic resinous products

Steam gasification of rapeseed, wood, sewage sludge and miscanthus biochars for the production of a hydrogen-rich syngas

Steam gasification of biochars has emerged as a promising method for generating syngas that is rich in hydrogen. In this study four biochars formed via intermediate pyrolysis (wood pellet, sewage sludge, rapeseed and miscanthus) were gasified in a quartz tubular reactor using steam. The dynamic behaviour of the process and effects of temperature, steam flow and particle size were studied. The results show that increases in both steam flow and temperature significantly increase the dry gas yield and carbon conversion, but hydrogen volume fraction decreases at higher temperatures whilst particle size has little effect on gaseous composition. The highest volume fraction of hydrogen, 58.7%, was obtained at 750 °C from the rapeseed biochar

Ultrasound-induced emulsification of subcritical carbon dioxide/water with and without surfactant as a strategy for enhanced mass transport

Pulsed ultrasound was used to disperse a biphasic mixture of CO2/H2O in a 1 dm3 high-pressure reactor at 30 °C/80 bar. A view cell positioned in-line with the sonic vessel allowed observation of a turbid emulsion which lasted approximately 30 min after ceasing sonication. Within the ultrasound reactor, simultaneous CO2-continuous and H2O-continuous environments were identified. The hydrolysis of benzoyl chloride was employed to show that at similar power intensities, comparable initial rates (1.6 ± 0.3 × 10–3 s–1 at 95 W cm–2) were obtained with those reported for a 87 cm3 reactor (1.8 ± 0.2 × 10–3 s–1 at 105 W cm–2), demonstrating the conservation of the physical effects of ultrasound in high-pressure systems (emulsification induced by the action of acoustic forces near an interface). A comparison of benzoyl chloride hydrolysis rates and benzaldehyde mass transport relative to the non-sonicated, ‘silent’ cases confirmed that the application of ultrasound achieved reaction rates which were over 200 times faster, by reducing the mass transport resistance between CO2 and H2O. The versatility of the system was further demonstrated by ultrasound-induced hydrolysis in the presence of the polysorbate surfactant, Tween, which formed a more uniform CO2/H2O emulsion that significantly increased benzoyl chloride hydrolysis rates. Finally, pulse rate was employed as a means of slowing down the rate of hydrolysis, further illustrating how ultrasound can be used as a valuable tool for controlling reactions in CO2/H2O solvent mixtures

Recovery and reuse of discontinuous carbon fibres by solvolysis: Realignment and properties of remanufactured materials

Discontinuous carbon fibre tows were recovered after solvolysis of an aeronautic type composite made with RTM6 epoxy resin. A Sohxlet extraction method was used to quantify the organic residue on the fibre tows and showed that less than 3 wt% was remaining on the surface. The recovered tows were therefore reused directly to manufacture a plate with randomly distributed carbon fibres and then three plates with realigned carbon fibres. The latter were then characterised and tested and the results obtained were compared to the material manufactured using the same type of virgin fibres by the same method. The materials made from recycled carbon fibres showed very good properties in comparison to the virgin fibre material, despite the presence of flaws such as quality of the fibre surface after solvolysis, alignment and voids). This is the first time in the open literature that carbon fibres recovered from solvolysis were reused in this way together with characterisation of the resulting materials

Current status of recycling of fibre reinforced polymers: Review of technologies, reuse and resulting properties

AbstractA complete review of the different techniques that have been developed to recycle fibre reinforced polymers is presented. The review also focuses on the reuse of valuable products recovered by different techniques, in particular the way that fibres have been reincorporated into new materials or applications and the main technological issues encountered. Recycled glass fibres can replace small amounts of virgin fibres in products but not at high enough concentrations to make their recycling economically and environmentally viable, if for example, thermolysis or solvolysis is used. Reclaimed carbon fibres from high-technology applications cannot be reincorporated in the same applications from which they were recovered, so new appropriate applications have to be developed in order to reuse the fibres. Materials incorporating recycled fibres exhibit specific mechanical properties because of the particular characteristics imparted by the fibres. The development of specific standards is therefore necessary, as well as efforts in the development of solutions that enable reusers to benefit from their reinforcement potential. The recovery and reuse of valuable products from resins are also considered, but also the development of recyclable thermoset resins. Finally, the economic and environmental aspects of recycling composite materials, based on Life Cycle Assessment, are discussed

Recycling carbon fibre with an acetone/water solvent and zinc chloride catalyst: resin degradation and fibre characterisation

The degradation of a carbon fibre reinforced epoxy resin with an acetone/water mixture and ZnCl2 catalyst was investigated. The solvent/catalyst system achieved a resin removal yield in excess of 94% after 1.5 h at 290°C and 45 min at 300°C. Single fibre tensile testing indicated an increase in fibre strength after the recycling process. The strongest fibres were recovered using a reaction temperature of 290°C and exhibited a strength of 3.21 ± 1.10 GPa. The technique developed therefore appears to recover high quality fibres while reducing the temperature by 30°C and process time by 25% when compared to earlier work

Supercritical fluid coating of API on excipient enhances drug release

A process to coat particles of active pharmaceutical ingredient (API) onto microcrystalline cellulose (MCC) excipient shows promise as a new way to dosage forms showing enhanced drug release. The process consists of a fluidized bed operated at elevated pressure in which API particles are precipitated from a Supercritical Anti-Solvent process (SAS). MCC particles were used as an excipient in the fluidized bed and collect the SAS-generated API particles. Naringin was selected as the model API to coat onto MCC. A number of operational parameters of the process were investigated: fluidization velocity, coating pressure, temperature, concentration of drug solution, drug solution flow rate, drug mass, organic solvent, MCC mass and size and CO2-to-organic solution ratio. SEM and SPM analyses showed that the MCC particle surfaces were covered with near-spherical nanoparticles with a diameter of approximately 100–200 nm, substantially smaller than the as-received API material. XRD showed that naringin changed from crystalline to amorphous during processing. The coated particles resulting from the SAS fluidized bed process have a higher loading of API, gave faster release rates and higher release ratios in comparison with those produced using a conventional fluidized bed coating process. The approach could be transferred to other industries where release is important such as agrochemical, cosmetic and food