Battelle - Chemical and Environmental Technology Process Optimization and Development


The historical focus of CET has been applying these sciences to challenges involving highly hazardous chemicals such as chemical warfare agents, organophosphates, thioethers, and arsenicals; however, as a result of dealing with the processing and disposal of these materials, the group has developed expertise in many other categories of chemicals.

CET staff routinely performs a wide range of chemical process and analytical chemistry services for clients. Our staff have started with a need for a new product and taken it through all the steps required for development, including preparation of the concept for a new chemical, synthesis of small amounts, measurement of physical properties, process reaction, laboratory process development, plant scale-up, and development of the analytical methods needed to verify its purity and the presence of by-products. In addition to chemical process and analytical chemistry services, CET staff team with other Battelle product providers to perform a wide range of equipment and materials testing.

The CET product line has over 600 professional staff located throughout the United States. Work is performed in Battelle and client-owned lab facilities that are either ISO 9001 registered or has pending registration.

Battelle Columbus Facility

Battelle Columbus Facility

CET Analytical Chemistry Capabilities

CET analytical chemistry staffs are highly trained professionals using state-of-the-art equipment and facilities to accomplish the chemical analysis needs of our customers. This includes development of analysis methods to determine the presence of specific chemical compounds in a variety of sample matrices; trace level analysis of samples for the presence of the compounds of interest; custom chemical synthesis of toxic and other specialized compounds; forensic analysis to characterize unknown materials or identify what compounds are present in a sample; and other chemistry support as needed. Specifically, our analytical chemistry groups perform:

  • Chemical synthesis
  • Analytical method development
  • Trace chemical analyses
  • Forensic analyses

Our staffs routinely conduct client and international proficiency tests, where we receive a variety of sample matrices that could contain literally anything. Our staffs quickly assess and analyze the samples and provide written documentation validating the findings.

A prime example of this capability is our forensic services in response to the Organization for the Prohibition of Chemical Weapons (OPCW) international proficiency tests. The OPCW provides three different sample matrices usually containing up to 10 analytes from thousands of possible compounds with the final report due no later than 14 calendar days from sample receipt. Our staff has one of the best overall ratings in these tests.

Battelle’s analytical chemistry equipment and facilities are world class and state-of-the-art. CET-owned analytical equipment is currently valued at over $10M and is continually replenished to preclude rapid obsolescence. A new laboratory facility with over 15,000 square feet of laboratory space is located in Columbus, Ohio and a 10,000 square foot laboratory was recently commissioned in Aberdeen, Maryland. Battelle also has access to many U.S. Government facilities through cooperative research agreements.

Chemical Process Development and Engineering

CET chemical engineers and scientists provide a wide range of process engineering and optimization services. Our expertise and research facilities enable us to provide reaction studies, data analysis, process modelling and scale-up design and pilot plant engineering. Battelle staff routinely work with extremely hazardous chemicals, including chemical warfare agents, and with non-hazardous materials at the laboratory, bench, and pilot scales.

Process Optimization at the Laboratory and Bench Scale

Our approach to process science and engineering is to integrate fundamental scientific principles into engineered systems to develop novel process systems that are efficient and cost-effective. Thus, novel concepts are evaluated and developed from both a basic science and an engineering perspective.

Teams of engineers with process scientists can take an idea from proof of concept, through lab evaluation, scale-up design and fabrication, to pilot-plant verification. These integrated teams use other resources as needed to assist in establishing the overall viability of a process.

Complementing the wide range of analytical tools provided by our analytical chemistry groups, our process chemists and engineers have been trained to use the Mettler RC1e reaction calorimeter and ASI ReactIR to support our reaction engineering and scale-up studies. These units stand alone, but are often used together to determine both the thermodynamic and kinetic properties of reactions. The Mettler RC1e reaction calorimeter is an advanced, computer-controlled system for studying and evaluating chemical reactions.

Process Optimization at the Laboratory

It is designed for investigation of liquid-liquid, liquid-solid, and liquid-gas reactions. It offers an optional distillation capability and can be operated in a batch, semi-batch, or continuous flow mode. It is routinely used to determine heats of reaction, adiabatic temperature rise, and specific heats of reactants and products.

It has safety features designed in to quench runaway reactions. The Mettler RC1e can be operated adiabatically, isothermally, or in a constant heat flux mode.

RC1e with in-situ ReactIR FT-IR Probe

The reactors at Battelle range from 1 liter to 5 liter, are made of glass or stainless steel, and are rated from atmospheric pressure up to 60 bar (less for glass reactors). Temperatures from –10-150 °C (–50 °C to 300 °C) can be obtained with add-on cooling or heating.

RC1e with in-situ ReactIR FT-IR Probe

To determine reaction rates and conversion, we use a combination of real-time, in-situ analysis of the reaction matrix and standard post-reaction product analyses. For real time analysis, CET staff uses the ASI ReactIR to analyze the reaction mass up to several times each minute.

FT-IR Real Time Output (Reversed) – Shows Increase/Decrease of Key Functional Groups vs. Reaction Time

This instrument is also the key to determining rates of reaction, conversion, and identifying intermediate reactions.

FT-IR Real Time Output

To aid process designersin conducting experimental sensitivity analysis, Battelle staff manipulates reaction data with specialized software. Many of Battelle’s scientists and engineers have been trained in and regularly use statistical design of experiment (DOE) methods, used for many process scale-up and process improvement projects.

Response Surface of a GB Decontamination Reaction

Process Design and Scale-up

In addition to process optimization studies, our researchers conduct a variety of process design, scale-up and modernization projects. As an example, Battelle conducted a series of experiments to optimize the formulation of a limited-tack, water-disperse adhesive.

After reaching optimization at the 1-liter size, Battelle was asked to scale up the reaction directly to 100 gallons to produce materials for a product test. Application of DOE procedures made it possible to produce the optimized reaction after two large-scale runs by using the response surfaces identified during the bench-scale testing.

Battelle has also optimized the reagents in a complex agent decontamination reaction by using EChip, a commercial DOE support software package. EChip helps Battelle staff conduct initial experimental planning and then optimize the process by recommending experiments to identify sensitive points on the curve, data outliers, and other sensitive areas.

Battelle also uses other software such as MathCad and Excel to support testing and evaluation projects. The preferred tool of Battelle engineers for process design is ChemCAD, a chemical process simulator. Battelle researchers routinely augment the database used in ChemCAD models to include its data collected during our Mettler runs and other laboratory tests. This provides designers with the most accurate simulation results.

Examples of Process Engineering Services

  • Process design of specialty chemical processes to evaluate the manufacturing by-products for a wide range of chemicals including organophosphates, ethers, thioethers, amines, and halogen-bearing chemicals
  • Use of chemical process models such as CHEMCad to develop preliminary process designs
  • Process reaction in tools such as the Mettler reactor to determine liquid physical properties and to safely study phenomena such as rapid polymerization
  • Production of monomers and polymers at laboratory and pilot scale for materials testing
  • Subscale process testing to determine process emissions
  • Scale-up of processes from bench-scale to several gallons per hour of production
  • Rapid prototyping of chemical process modules and pilot plants.

Battelle can help you evaluate different process approaches; test selected process approaches to evaluate safety, emissions, and process bottlenecks; and scale up processes from laboratory scale to a pilot plant scale.

Scale-Up of Hydrolysis Reaction System

Battelle regularly teams with vendors to produce a high-quality, skid-mounted or stand-alone process to produce chemicals of interest for its clients.

Scale-Up of Hydrolysis Reaction System to 20 Gallons/Hour

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