Process Intensification: A Prerequisite for Success in Custom Manufacturing Chemspec 2016, Basel Dr. Christoph Schaffrath Dr. Guido Giffels Slide 1 June 1st, 2016
Saltigo Who are we and where do we come from? A globally operating company for exclusive synthesis and innovative fine chemicals Saltigo profile customers: ca. 150 Core competence employees: ca. 1.250 products/projects: ca. 400 Since 2006 10 production plants Market-orientated, Saltigo – a company Leverkusen + Dormagen (Ger) custom manufacturing of the LANXESS service provider group Lanxess profile spin off from Bayer 2004 2005-2006 employees: 16,225 Business Unit Outsourcing partner Fine Chemicals for fine chemicals sales: € 7.9 billion in 2015 of LANXESS global footprint: 29 countries 52 production sites Chemspec Basel 2016, Saltigo Presentation Slide 2 June 1st, 2016
Saltigo – A global player in custom manufacturing serving different industries Exclusive production 100 - 5.000 kg/a Intermediates and APIs Pharmaceuticals Regulated area (CGMP, etc.) Custom Manufacturing Production volumes > 1.000 t/a Agro chemicals Intermediates and AIs Regulated area (Biocides Regulation, etc.) Often non-exclusive products Fine chemicals ISO-production or special demands Chemspec Basel 2016, Saltigo Presentation Slide 3 June 1st, 2016
Focus on market oriented services: Support of customer needs along the complete project lifecycle Advanced Raw Material Active Substance Formulation Customer Intermediate Process Idea Lab Pilotation Market Production development Core competence of Saltigo Custom-made process development Custom manufacturing/synthesis up to 5,000 t/a Efficient project management Enhanced service support (registration, analytics, etc.) Continuous improvement process Professional procurement, reliable supply chain Process Intensification: A prerequisite for successful custom manufacturing Chemspec Basel 2016, Saltigo Presentation Slide 4 June 1st, 2016
Process intensifications drive efficiency and cost optimization A diverse toolbox is required for a successful implementation Project Management Debottlenecking Data Generation Capacity Innovation Process Plants Development Continuous Teams Process Process Intensification Mindset Improvement Customer Analytics Technology QA and QC Economy Investments Milestones and Implementation Chemspec Basel 2016, Saltigo Presentation Slide 5 June 1st, 2016
Process intensifications – What does it mean? „Getting More out of Less“ Chemspec Basel 2016, Saltigo Presentation Slide 6 June 1st, 2016
Getting More out of Less – How? Ways to achieve this goal 1. More „ Right 1 st Time “, optimizing process & parameters to improve product quality, reducing/omitting number of process steps, reworks, … 2. Changing Equipment (Hardware) improve setup 3. Higher Space-Time-Yields by Process Optimization, e.g. shortening cycle time, increasing output/batch etc. Chemspec Basel 2016, Saltigo Presentation Slide 7 June 1st, 2016
Process Intensification 3 Case studies Increasing the bulk density of an agrochemical product Case #1 by using multivariate data analysis Significant increase of production capacity & productivity Case #2 by stepwise modification of reactor setup Shortening cycle time of an exothermic reaction Case #3 by use of an intelligent control factor Titel /as Folie 8 19.05.2016
Case Study #1 Objective: increase the bulk density of a crystallized product Case description Large-scale custom-made product crystallizes in (at least) 2 polymorphorphic modifications Customer requires Mod. B , a defined purity (specification!) and a high bulk density Mod. B Mod. A Crystallizes kinetically controlled („faster“) Thermodynamically more stable, may be formed out of Mod. A Gives better & required purity Required product form by the customer Mechanically less stable Gives lower purity if crystallized directly Grinding during drying leads to low particle size and to low bulk density Mechanically more stable, larger particle size Bulk density is crucial, as a certain amount of Gives higher bulk density product per big bag is asked by the customer Chemspec Basel 2016, Saltigo Presentation Slide 9 June 1st, 2016
Case Study #1 Objective: increase the bulk density of a crystallized product Objective: How to get… the right modification (Mod. B) ? • the right purity ? • a good bulk density ? • … with a mimimum of effort? „Is this the best option?“ Crystallize Mod. B directly: Purity not sufficient Crystallize A first, isolate & recrystallize, seeding B: V Let‘s look Works, but additional (re)crystallisation (= effort) deeper into this one Convert Mod. A Mod. B on the dryer ? Possible, but drying process gave varying results Chemspec Basel 2016, Saltigo Presentation Slide 10 June 1st, 2016
Case Study #1: Multivariate Data Analysis – Tool to pick the right parameters and values Multivariate Data Analysis – Drying Process normalized data showing effect on bulk density Thermal impact triggers the modification change from Mod. A Mod. B Data Parts 1-2 v03.M11 (OPLS)(BLM) E10 P80A Sources of Variation Drying Process (not automated) gave P80B Colored according to Var ID ($SourceID) P81 various results in bulk density Pressure Einsatz aus F2929 Inertisieren Evakuieren Kühlen Belüften Trocknen Ende Austragen R15Y R60Y Temperature R85Y Multivariate Data Analysis „highlighted“ the 0,02 S10 T10 crucial process parameters during drying: T60 0,01 T61 Pressure (vacuum) – higher pressure in T80 T81 p[1] 0 the beginning is better -0,01 Bulk temperature – higher temperature in the beginning is better -0,02 Energy input Energy application (by stirrer): -0,03 Charging Drying Cool, areate, discharge lower is better – grinding! 0 36 73 109 146 189 294 10 10 42 74 106 138 170 205 251 306 367 665 34 0 62 9 47 86 175 Var ID ($MaturityID) Parameter data from approx. 60 batches R2X[1] = 0,111 SIMCA 14.1 - 2016-02-18 15:10:14 (UTC+1) high amplitude = large impact on bulk density Chemspec Basel 2016, Saltigo Presentation Slide 11 June 1st, 2016
Case Study #1: Increase Product Bulk Density Rationale behind the “right” parameters Possible „Routes“ Rationale A-wet A-dry B-dry: grinding of Mod A during drying low bulk density ? V A-wet B-wet B-dry: formation of stable Mod B first, then drying, larger particles and higher bulk density First tempering the wet product at higher pressure („bad“ vacuum) and resulting higher inner temperature leads to fast change from Mod. A Mod. B = less grinding of mechanically less stable Mod. A, resulting in a better bulk density after drying. Chemspec Basel 2016, Saltigo Presentation Slide 12 June 1st, 2016
Case Study #1: Increase Product Bulk Density Results after optimization Bulk Density before/after Optimization Summary Relevant process parameters were identified by means of multivariate data analysis Histogram of Bulk density 25 Significant increase of bulk density was achieved 20 Requested amount of product per big bag can 15 be filled Before Optimization Part 1 Optimized Part 2 10 5 0 7 9 1 3 5 7 9 1 3 5 7 9 1 3 5 7 9 1 3 5 7 9 1 3 5 7 9 2 2 3 3 3 3 3 4 4 4 4 4 5 5 5 5 5 6 6 6 6 6 7 7 7 7 7 , , , , , , , , , , , , , , , , , , , , , , , , , , , 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Chemspec Basel 2016, Saltigo Presentation Slide 13 June 1st, 2016
Case Study #2: Increasing Capacity & Productivity by Optimized Reactor Setup Chemspec Basel 2016, Saltigo Presentation Slide 14 June 1st, 2016
Case Study #2 Increasing capacity & productivity by optimized reactor setup Case description Large scale chlorination product (B) was produced in batch mode with limited capacity (A) reacts to target product (B). (B) reacts further to byproduct (C) in a consecutive reac-tion. To maximize selectivity, (A) is only partially converted and recycled during workup Objective : increase capacity / productivity to meet market demand Cl 2 Cl 2 A B C Bottleneck Target Product Chemspec Basel 2016, Saltigo Presentation Slide 15 June 1st, 2016
Case Study #2 Increasing capacity & productivity by optimized reactor setup Szenario 2): First expansion Add 2 nd distillation unit (A) Change to continuous operation of distillation: Unit 1: recycle (A) Unit 2: isolate product (B) (B) Doubling chlorination unit Bottleneck Cl 2 Cl 2 A B C continuous (C) Chemspec Basel 2016, Saltigo Presentation Slide 16 June 1st, 2016
Case Study #2 Increasing capacity & productivity by optimized reactor setup Szenario 3): Debottlenecking distillation (A) Bottleneck Reactor setup as szenario 2, plus … Improved column for distillation unit 1 (B) Cl 2 Cl 2 A B C continuous continuous (C) Chemspec Basel 2016, Saltigo Presentation Slide 17 June 1st, 2016
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