Automated Reaction Calorimeter

Heat balance analysis

Comprehensive consideration of heat transfer and heat dissipation in calorimetric processes, over the entire temperature range- Full liquid level range system thermal capacity calibration 

High-precision temperature control

High performance dynamic circulating oil bath with an accuracy of ±0.1K over the entire temperature range 

Intelligent Control

Automatic sampling and feeding, automatic cutting off of the sampling power supply in an emergency to ensure the safety of the reaction system 

Flexible customization

Flexible component matching, rich software functions, and diverse control processes 

Product Features

For the complex and changeable synthetic reaction processes in the fields of fine chemicals and pharmaceuticals, the reaction calorimeter canmeasure the real-time exothermic heat flow of the reaction system in the reactor to obtain thermal behavior information such as the total heat release, specific heat release, real-time heat conversion rate and material accumulation of the reaction, and calculate the adiabatic temperature rise of the target reaction and the maximum temperature (MTSR) that the system can reach after loss of control. Based on this, the severity of the reaction loss of control and the level of process hazard are evaluated, providing a basis for process optimization and scale-up of the target reaction.Supports heat flow calorimetry, power compensation calorimetry, and evaporation reflux calorimetrySupports multiple temperature control modes such as isothermal, constant temperature, scanning, etc.Real-time display of test status such as kettle temperature, jacket temperature, feed quality, etc.With peripheral database, one system supports multiple reactors interchangeableKey parameters and status safety thresholds can be set, and "one-button" rapid cooling, abnormal status alarm and automatic shutdown are available when the reaction is out of control 

Structure

Accurate, reliable calorimetry performance

Mixer

The drive speed can be set automatically or manually remotelyNormal pressure reactor with mechanical stirrer, medium/high pressure reactor with magnetic stirrer

Injection pump

Metering pump for liquid sample injection control, which can be controlled by monitoring system

Reactor

A variety of materials and specifications of reactors are available, including Glass, 316 Stainless steel, and Hastelloy C276 . Double reactor reaction calorimeters can also be customized according to requirements. The instrument shown on the right is RC HP-100OD double reactor automatic reaction calorimeter

Central control cabinet

Contains a core control unit that collects component working status in real time, monitors key temperature signals, and achieves high-precision temperature control

Circulation oil

Provides the power required for rapid heating or cooling, and uses the heat transfer medium to circulate through the reactor to control its temperature

Mode   

Adapt to various calorimetric methods, reliable and accurate 

1. Heat flow method

Heat flow calorimetry can accurately determine the specific heat capacity of the sample and the heat transfer factor between the sample and the reactor jacket through a calibration process, and measure the temperature difference between the sample and the jacket in real time during the reaction process, and calculate the real-time heat release heat flow of the sample. The heat flow method can obtain more accurate calorimetric data. 

2. Power compensation method

Power compensation calorimetry uses a calibrated heater to provide a certain background power to maintain the entire system in thermal equilibrium. During the reaction, the real-time heat release heat flow of the sample is calculated by measuring the change in heater power. The power compensation method can be used to conduct experiments more efficiently. 

3. Evaporation Reflux Method

Reflux (distillation) calorimetry can determine the specific heat capacity of the sample, the heat transfer factor between the condenser and the refrigerant, and between the sample and the reactor jacket through the calibration process, and measure the temperature difference between the inlet and outlet of the condenser and between the sample and the jacket in real time during the reaction process, and calculate the real-time heat release heat flow of the sample. When the reaction is carried out under boiling conditions, the reflux mode calorimetry is required. 

Software

Simple, fast and convenient analysis software

Parameter calculation

ΔH = r /m

m is the total mass of the reactants  

Heat conversion rate: a% = H t /H total

H t from the start of the reaction to the time t Total heat release

H total The total heat released from the start to the end of the reaction  

Material accumulation: X acc r /ma) · 100%dm r Feeding rate 

Maximum temperature of thermal runaway system:

MTSR=T p + r /(Cp·

m total ) ·X acc T pProcess temperaturem total 

Total mass of reaction system

Risk Assessment Report

Reaction risk assessment

Working Guidance and Annexes: 

Fine Chemicals

Safety Risk Assessment Guidelines (Trial)

It is required to evaluate the hazard level of the reaction based on parameters such as reaction heat and adiabatic temperature rise, evaluate the possibility of reaction runaway based on parameters such as maximum reaction rate arrival time, conduct multi-factor hazard assessment in combination with relevant reaction temperature parameters, and determine the hazard level of the reaction process.

Data analysis

Visual interface

It is convenient to realize experimental process editing, system parameter adjustment, Remote firmware update and other functions.

T set

Target temperature T r  

Sample temperature Tj

Jacket temperature

T r -T jDifference between sample temperature and jacket temperature

U Calibrate heating power supply voltage 

I Calibrated heating power supply current 

P  Pressure in reactor

UA Heat transfer factor between sample and jacket

Quickly obtain characteristic parameters

Reaction heat flowHeat transfer factor

Sample specific heat capacity System heat dissipation Total heat release

Specific exothermic enthalpy Adiabatic temperature rise MTSR

Maximum material accumulation rate

Multi-parameter combination

The monitoring system automatically saves the acquired data and imports it into the analysis software for data analysis after the test is completed. Quick analysis and combination are used for calorimetric and in-situ detection data (heat flow curve, molecular spectrum, viscosity, etc.) to study the reaction process.

Application Cases

Help you assess risks and optimize processes 

Accurate calorimetry for temperature-dependent reactions

Variable temperature reactions are very common in industrial production, and many reactions may require multiple temperature changes. The difficulty of variable temperature reaction calorimetry is that the thermal characteristic parameters and heat dissipation of the reactor system continue to change during the reaction, affecting the reaction heat flow calculation. 

Model No: ERC uses full temperature range system heat capacity correction technology and flexible baseline correction

The method addresses the above problems. Whether it is an exothermic reaction diagram (a) or an endothermic exothermic diagram (b), it can obtain an accurate and ideal reaction heat flow curve, helping users optimize process conditions such as start and end temperatures and heating rates, and can also perform reaction kinetics analysis. Suzuki coupling reaction of phenylboronic acid and bromoaniline: the reactants are added at once, the temperature is controlled at 25℃, the palladium catalyst is added, and then the temperature is raised to 72℃ at a uniform rate. Normal pressure reactor, heat flow calorimetry.

Three-file tin synthesis, format reaction, reactants are put in at once at room temperature, the reaction temperature is raised to 95℃ at 0.7℃/min, kept at this temperature for 10min, and then raised to 115℃ at 0.4℃/min. High-pressure reactor, heat flow calorimetry.

Synthesis of dry strength agent - calorimetry of highly exothermic reaction

Typical polymerization reactions are characterized by strong heat release and high viscosity, which poses challenges to the precise temperature control and heat measurement during the reaction process. The figure shows the polymerization reaction of acrylamide. After the initiator is added, the reaction immediately begins to release heat violently, with the maximum heat release rate reaching about 600 W. Once the reaction gets out of control, the maximum process temperature MTSR can reach 256°C.

Model No: ERC uses a jacketed oil bath for efficient cooling, which can quickly adjust the reaction temperature, effectively suppress overheating, avoid runaway temperatures that may cause material rushing and explosion, and ensure experimental safety.

Synthesis of a platelet inhibitor (Tiganovol) - calorimetry combined with in situ MIR technologyThe combination ofModel No: ERC and in-situ MIR can quickly and effectively monitor the reaction process and determine the reaction termination point, thereby optimizing the process parameters such as reaction time and temperature. The process before the optimization of a drug synthesis reaction is divided into two stages. First, the base material is added at 2°C, and the catalyst is slowly added to initiate the reaction; after the catalyst is added, the temperature is raised to 22°C and the reaction is kept warm for 3 hours.

In Figure (a), the calorimetric results show that the reaction heat flow has approached 0 before the temperature is raised, indicating that the reaction has been basically completed; in Figure (b), the real-time data obtained by in-situ MIR can confirm the calorimetric results, and it can be found that the characteristic absorption peak of the product has stabilized before the catalyst feeding is completed. The above results all show that the insulation stage has almost no effect on improving the reaction conversion rate.

Based on the above conclusions, the drug manufacturer reduced the insulation reaction time from 3 hours to 1 hour, significantly improving production efficiency while ensuring product quality.

Technical specifications

Model No: ERC Series Automated Reaction Calorimeter

Calorimetric method: heat flow method, power compensation method (optional), reflow method (optional)

Customized Reactor

Temperature control

Power Control

Injection system

 Other parameters