RC1 Reaction Calorimeter 自动实验室反应器说明书

The RC1 Reaction Calorimeter With the RC1 the course of a chemical reaction or a physical transformation is followed with regard to heat change, viscosity,yield, quality and other process parameters. The data obtained form the basis for the planning of pro-duction facilities and the optimiza-tion of processes regarding safety,economic viability and ecology.But the determination of process parameters is not the only important feature; the RC1 is also an auto-matic laboratory reactor. It can be used to perform and repeat experi-ments once or several times in the same manner or with systematically changed experimental parameters.Processes can thus be investigated simply and dependably to obtain an in-depth knowledge of their characteristics.
The heat balancing
The RC1 allows generation of a complete heat and mass balance over the entire process. The heat exchange across the reactor wall is determined and is a measure of the heat effects of all chemical reactions and physical transformations occurring in the reactor.
Distilling and refluxing with the
RC1 Reaction Calorimeter.
Distillation and Reflux Set
Glass apparatus:
1Receiver, 1 liter
2Bent adapter, insulated, silver coated
3Product condenser
4Electromagnet for swing-out funnel
5Reflux divider, insulated, silver coated
6Condenser, insulated, silver coated
7∆T cond measurement,
coolant inlet and outlet
8Vacuum connection, condenser
9Pt100 temperature sensor
for liquid phase
10Pt100 temperature sensor
for gas phase
The distillation and reflux set can simply be
mounted on the various reactors of the
RC1. The standard connections allow
expansion of the system with other
commercially available glass equipment
and parts.
The measurement principle
The transformed energy and hence the heat dissipated by the reflux condenser is determined by means of the coolant circulating in the con-denser. This calculation involves multiplying the temperature differ-ence ∆T cond measured between the coolant inlet and outlet by the spe-cific heat and the constant mass flow of the coolant.The distillation and reflux set
as an accessory for the RC1
The accessory kit includes all nec-essary glassware, the sensors for measuring the temperature differ-ence ∆T cond, the flow controller of the coolant and the required instal-lation and assembly material. The glass apparatus comprises
a condenser, a reflux divider with electromagnetically controlled swing-out funnel for diverting the returning condensate and a bent adapter for the reactor cover.
To ensure optimum thermal insula-tion, all parts mentioned above are vacuum insulated and mirrored.
Distillation and work under reflux Chemical reactions are frequently performed at the boiling point of the solvent. The heat of reaction released is dissipated via the reflux condenser of the reactor. The heat dissipated in the condenser is not taken into account in the heat ba-lancing across the reactor wall and is therefore determined separately
in the distillation and reflux set.
In the process development phase, working under reflux with simulta-neous heat balancing allows experi-mentation under realistic conditions, in other words the future production conditions.
With the electrically operated swing-out
funnel, the reflux ratio can be controlled
and manual or automatic switching
between distillation and reflux effected. 8
7
6
5
4
3
10
9
2
1
To allow observation of the vapor
and liquid flows, the condenser
and the reflux divider have small
windows, i.e. nonmirrored areas.
Other glass parts are the product
condenser and a 1-liter receiver.
The setup is also suitable for work
under vacuum.
The connections between the
individual glass parts comprise
standard connectors and can read-
ily be combined with common
commercially available columns,
condensers and phase separators.
The flow controller
for the coolant flow
The differential pressure controller
keeps the flow rate constant even if
the coolant pressure varies on the
inlet side.
The reflux divider
The reflux divider is so constructed
that the temperature of the ascend-
ing vapor and that of the returning
condensate can each be measured
using a Pt100 sensor.
The integrated electromagnetically
operated swing-out funnel allows
either distillation or refluxing. The
swing-out funnel is controlled by
the RD10 Dosing Controller and
can be operated manually or pre-
programmed automatically during
the experiment. Periodic on/off
switching of the electromagnet
allows the desired reflux ratio to
be set between 0.1 and 0.9.
After cooling in the product
condenser, the distillate can be
collected in a receiver or led off
to a balance to determine its mass.
The measured values stored by the
balance are automatically used in
the mass balance calculation of
the reactor.
Measurement of ∆T cond
at the condenser
The ∆T cond sensor comprises two
temperature measurement probes
one of which is attached to the
coolant inlet while the other is
attached to the coolant outlet. The
∆T cond signal is transmitted via one
of the analog inputs of the RD10
Dosing Controller to the PC, where it
is stored and later plotted.
Calculation of Q r
under reflux conditions
The principle of the calorimetric cal-culations is based on the mass and heat balance of the reactor. The cal-culation is performed offline with the PC software WinRC. The heat balance comprises various terms which can be calculated indivi-dually or as totals. The two Q add terms are suitable for linear mea-surement systems and are freely programmable.
001:45:00001:47.30001:50:00001:52:30001:55:00001:57:30002:00:00002:02:30002:05:00002:07:30002:10:00002:12:30002:15:00002:17:3
0002:20:00002:22:30002:25:00002:27:30002:30:00002:32:30002:35:00002:37:30002:40:00002:42:30002:45:00002:47.30002:50:00002:52:30002:55:00002:57:30003:00:00003:02:30003:05:00003:07:30003:10:00003:12:30003:15:00003:17:30003:20:00003:22:30003:25:00003:27:30003:30:00003:32:30003:35:00003:37:30003:40:00
Pen 4
Pen 7
Pen 9
5
4
Pen 2
Pen 1
Pen 6
3
2
1
T r B 2
∆T Kond Q r
T v
T i
Examples: Saponification of methyl benzoate under reflux at pH > 10. The curves show a section from the experimental profile:1Isothermal phase at Tr = 90°C
2Changeover to refluxing; Tj (Pen 6) is controlled to 15 K above Tr (Pen 1): the temperature of the reaction mass is raised to the boiling point.
3Following heating of the reactor cover and the glass connections, the water vapor first reaches the temperature sensor for the vapor temperature (Tv, Pen 2), it then condenses in the condenser and this is shown by the experimental signal ∆T cond (Pen 7).
4The calibration heating is switched on for 10 min; the additional quantity of heat introduced generates additional vapor and hence increased condenser cooling power.
5One mole (136 g) of methyl benzoate is added over a period of 15 min (curve B2, Pen 4). The heat of reaction is again dissipated via the vapor. The boiling temperature (Tr, Pen 1) is lowered by the reaction product methanol.
The heat production rate (Qr, Pen 9) is calculated from the experimental signals in accordance with the heat balance equation.
T j reactor jacket temperature T r reaction mass temperature T v
vapor temperature below the condenser Q r heat production rate ∆T cond temperature difference
at condenser
B 2added amount of reagent
Subject to technical changes
© 10/04 Mettler-Toledo AG, 51724746.P&D MarCom Schwerzenbach.
Printed ind Switzerland on 100% chlorinefree paper, for the sake of our environment.
Mettler-Toledo Inc., AutoChem, Inc.7075 Samuel Morse Drive Columbia, MD 21046, USA Phone 410 910 8100Fax 410 910 8101Internet:
Mettler-Toledo GmbH, Reaction Engineering Sonnenbergstrasse 74
CH-8603 Schwerzenbach, Switzerland Phone ++41 44 806 77 11Fax ++41 44 806 72 90Internet or。