Periodic Reporting for period 2 - NanoPAT (Process Analytical Technologies for Industrial Nanoparticle Production)
Période du rapport: 2021-12-01 au 2023-05-31
NanoPAT project will bridge this gap using three novel, complementary real-time in situ particle size characterization technologies – Photon Density Wave spectroscopy (PDW), Optofluidic force induction (OF2i) and Turbidity spectrometry (TUS). These technologies will be advanced from TRL 4 to a technology demonstration level for inline/online process monitoring at TRL 6 of the NanoPAT industrial partners. The objectives of the project are summarized in thirteen points.
To define the specifications of the processes to be monitored via the tailored NanoPAT technologies
To develop an inline monitoring tool based on PDW for the real time characterization of polymer dispersions, nano-silica and zeolite NPs
To develop an online monitoring tool based on OF2i for the characterization of hydroxyapatite and ceramic NPs
To develop monitoring tool based on TUS for the nano-characterization of silica, ceramic NPs suspensions in electrolytes and polymer dispersions
To deliver a PAT Platform for holistic digital process data storage and analysis
To design innovative data elaboration techniques for PAT applications
To set up the most suitable nano-characterization integrated solution for the production of polymer dispersions in DSM/COVESTRO
To set up the tailored nano-characterization integrated solution for the production of silica nanoparticles in EVONIK
To set up the tailored nano-characterization integrated solution for zeolites production in ARK
To set up the tailored nano-characterization integrated solution for the production of nano-hydroxyapatite in FLU
To set up the combined nano-monitoring technology to the semi-industrial electroplating pilot line in CNANO
To maximise the dissemination and innovation of NANOPAT outcomes through Open Innovation to benefit the NANOPAT consortium and the wider European process industry and Academia
To maximize the impacts of NanoPAT, including growth and job creation, via post project industrial commercialization of the project outcomes
To define the specifications of the processes to be monitored via the tailored NanoPAT technologies
To develop an inline monitoring tool based on PDW for the real time characterization of polymer dispersions, nano-silica and zeolite NPs
To develop an online monitoring tool based on OF2i for the characterization of hydroxyapatite and ceramic NPs
To develop monitoring tool based on TUS for the nano-characterization of silica, ceramic NPs suspensions in electrolytes and polymer dispersions
To deliver a PAT Platform for holistic digital process data storage and analysis
To design innovative data elaboration techniques for PAT applications
To set up the most suitable nano-characterization integrated solution for the production of polymer dispersions in DSM/COVESTRO
To set up the tailored nano-characterization integrated solution for the production of silica nanoparticles in EVONIK
To set up the tailored nano-characterization integrated solution for zeolites production in ARK
To set up the tailored nano-characterization integrated solution for the production of nano-hydroxyapatite in FLU
To set up the combined nano-monitoring technology to the semi-industrial electroplating pilot line in CNANO
To maximise the dissemination and innovation of NANOPAT outcomes through Open Innovation to benefit the NANOPAT consortium and the wider European process industry and Academia
To maximize the impacts of NanoPAT, including growth and job creation, via post project industrial commercialization of the project outcomes
To evaluate the performance of the three novel PATs in monitoring the synthesis in the different case studies, the industrial manufacturing processes were successfully replicated at lab-scale by the RTOs of the NANOPAT consortium (UPV: polymeric nanoparticles, UP: silica nanoparticles, MUG: nano-hydroxyapatite, ZHAW: zeolites, MUG: ceramic NPs electrolyte suspensions). Each RTO was equipped with their according PAT instruments (PDW: polymer dispersions, nano-silica and zeolite NPs; OF2i: hydroxyapatite and ceramic NPs; TUS: silica, ceramic NPs, polymer dispersions). Importantly, critical phases of different industrial processes have been distinguished. The monitoring of the evolution of particle size in the nano scale has for some cases been demonstrated and for others measures to achieve this have been identified and are currently being implemented. These achievements are supported by the effective utilisation of appropriate reference technologies. The traceability of the OF2i system has been greatly strengthened. The PDW and TUS probes, in the absence of specific national or European guidelines dedicated to inline nano characterisation, have been referenced by methods according to the requirements of the industrial processes and in accordance with guidelines for offline methods such as the OECD Test Guideline no. 125. Additionally, the specifications for upscaling the use cases have been defined.
The instrument hardware and measurement capabilities along with their software and documentation have been better adapted to the needs of the industrial partners on the basis of intensive pilot scale testing. The selected wavelengths and the dimensions of the PDW probe have been optimised. The OF2i technology has taken a major step towards sample-independent equipment validation routines and the stability of the measuring cell has been increased to deal with air bubbles. Also, the software has been expanded for nanoparticles with higher refractive indices. The hardware and software of the TUS system has been successfully modified to enable automatic dilution and demonstrated the potential for feedback control during the electroplating process. (WP2, WP3, WP4).
ADSC and IRIS have continued the development of a digital platform that stores, combines, and processes the monitoring data of the respective PATs for each case study to achieve maximum data exploitation. The viability for integrating at least two the PAT instruments has been shown. They have also implemented Computational Fluid Dynamics (CFD) studies for the correct location of each of the measuring devices within the case studies and for scale-up procedures later in the project. In two of the cases, the CFD studies have provided recommendations to increase process efficiency. For production of zeolites, the potential for reduction in agitation speed, including a modification of the mixing technology, was demonstrated. For the case of electroplating, the CFD pointed towards an increase in mixing efficiency via changing the inlet position. Many of the studies have yielded valuable information on sensor placement.
A summary of the deployment of the PAT instruments involved in the project (PDW, TUS, OF2i) in the five case studies has been generated. This includes a statement of each end user commenting on the suitability of each PAT for their case study. This deliverable aims to inform the public about the current state of the project, emphasising the potential impact the knowledge and technology transfer of NanoPAT may have on large industrial companies and, therefore, the European economy (WP6).
The instrument hardware and measurement capabilities along with their software and documentation have been better adapted to the needs of the industrial partners on the basis of intensive pilot scale testing. The selected wavelengths and the dimensions of the PDW probe have been optimised. The OF2i technology has taken a major step towards sample-independent equipment validation routines and the stability of the measuring cell has been increased to deal with air bubbles. Also, the software has been expanded for nanoparticles with higher refractive indices. The hardware and software of the TUS system has been successfully modified to enable automatic dilution and demonstrated the potential for feedback control during the electroplating process. (WP2, WP3, WP4).
ADSC and IRIS have continued the development of a digital platform that stores, combines, and processes the monitoring data of the respective PATs for each case study to achieve maximum data exploitation. The viability for integrating at least two the PAT instruments has been shown. They have also implemented Computational Fluid Dynamics (CFD) studies for the correct location of each of the measuring devices within the case studies and for scale-up procedures later in the project. In two of the cases, the CFD studies have provided recommendations to increase process efficiency. For production of zeolites, the potential for reduction in agitation speed, including a modification of the mixing technology, was demonstrated. For the case of electroplating, the CFD pointed towards an increase in mixing efficiency via changing the inlet position. Many of the studies have yielded valuable information on sensor placement.
A summary of the deployment of the PAT instruments involved in the project (PDW, TUS, OF2i) in the five case studies has been generated. This includes a statement of each end user commenting on the suitability of each PAT for their case study. This deliverable aims to inform the public about the current state of the project, emphasising the potential impact the knowledge and technology transfer of NanoPAT may have on large industrial companies and, therefore, the European economy (WP6).
FLUIDINOVA:
During the second reporting period, FLU worked in close collaboration with the partners from MUG and BRAVE for the production and characterization of the hydroxyapatite nanoparticles. The lab test rig setup developed by FLU allowed the partners from MUG to produce the hydroxyapatite nanoparticles in a reproducible way, simulating the industrial conditions for the characterization of the nano-hydroxyapatite using the OF2i technology.
COVESTRO
In the second reporting period, Covestro worked mainly on both the PDW and the TUS. Together with the TUS team, offline measurements where done.
EVONIK
During the second reporting period EVONIK has performed a number of implementation trials in a first measurement campaign at the laboratory with the PDWS. It has proven the industrial feasibility and process robustness of the PDWS.
The implementation work with the TUS sensor in cooperation with UP is showing significant progress and a first measurement campaign at the laboratory will start soon.
ARKEMA
During the second reporting period, ARKEMA has supported the synthesis trials of zeolite NaA and NaX at ZHAW. Industrial bulk chemicals were provided. Zeolite samples were also sent by ZHAW and characterised to validate the quality of the product according to the parameters established (crystallinity, purity and particle size distribution). In parallel, the selection of the pilot reactor for the extrapolation of PDWS was done, together with the definition of the adapter for the probe.
CNANO
CNANO performed a number of experiments to compare DLS, the method currently used by CNANO in house for measuring the particle size of ceramic NPs in electrolyte baths, with TUS and Of2i methods, developed in the frame of NanoPAT by IRIS and BRAVE, respectively.
During the second reporting period, FLU worked in close collaboration with the partners from MUG and BRAVE for the production and characterization of the hydroxyapatite nanoparticles. The lab test rig setup developed by FLU allowed the partners from MUG to produce the hydroxyapatite nanoparticles in a reproducible way, simulating the industrial conditions for the characterization of the nano-hydroxyapatite using the OF2i technology.
COVESTRO
In the second reporting period, Covestro worked mainly on both the PDW and the TUS. Together with the TUS team, offline measurements where done.
EVONIK
During the second reporting period EVONIK has performed a number of implementation trials in a first measurement campaign at the laboratory with the PDWS. It has proven the industrial feasibility and process robustness of the PDWS.
The implementation work with the TUS sensor in cooperation with UP is showing significant progress and a first measurement campaign at the laboratory will start soon.
ARKEMA
During the second reporting period, ARKEMA has supported the synthesis trials of zeolite NaA and NaX at ZHAW. Industrial bulk chemicals were provided. Zeolite samples were also sent by ZHAW and characterised to validate the quality of the product according to the parameters established (crystallinity, purity and particle size distribution). In parallel, the selection of the pilot reactor for the extrapolation of PDWS was done, together with the definition of the adapter for the probe.
CNANO
CNANO performed a number of experiments to compare DLS, the method currently used by CNANO in house for measuring the particle size of ceramic NPs in electrolyte baths, with TUS and Of2i methods, developed in the frame of NanoPAT by IRIS and BRAVE, respectively.