DE1963975A1 - Device for recording, controlling or regulating chemical reactions in processes with energy toning - Google Patents

Description

Device for recording, controlling or regulating chemical reactions in processes with energy tint.

The invention relates to a device for detecting, controlling or rules of energy, such as B. Amounts of heat that are added or released during chemical processes (endothermic reactions) (exothermic reactions) and follow time laws with regard to the conversion of the reactants.

Previously, if you wanted to manufacture a product from a reaction mixture, so you had to know the reaction conditions in terms of time and temperature for the respective reactant mixture, if one to wanted to come to an equivalent end product with the same yield. The working conditions were usually determined so that you can first take samples under different working conditions, such as. B. Change in temperature and / or time and checked their characteristics, thus optimizing the process for transferring the test to manufacturing. This transfer the laboratory values av.f the fabrication was difficult. In most cases, different batches and different reaction vessels were used the end. The heat treatment and thus the sales conditions changed significantly with different dimensions. This became a Transfer to other scales is very complex.

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A device was invented which has an energy meter and a sensor which records the characteristic data determined in the experiment and controls or regulates the process via these characteristic data. In principle, the energy conversion is linked to the material conversion, from which the equivalence of the products is recognized The device is essentially geared towards taking the temperature or other physical data from the reaction mixture and measuring it, representing and counting these measured values as an amount of energy by suitable conversion using various elements, such as a multiplier. With the help of the recorded amounts of energy, which can also be used for analytical statements, the process can be controlled or regulated via suitable circuitry, for example one can intervene in the process with the various amounts of energy in order to achieve certain properties of the product. The intervention can take place automatically via the circuit These different amounts of energy show an actual state during an examination.

Examples are given below for the structural conditions of the sensor, counter, multiplier and circuit.

This method is based on the principle of recording the reaction turnover via the energy turnover and thus making it controllable. Furthermore, an analytical statement regarding the uniformity of the starting substances can be made from the determination of the amount of energy do.

So one becomes in the reactant mixture at the most unfavorable for the process Place, in order to ensure complete conversion here, too, insert a sensor and the measured values via a conversion device convert it into an amount of energy. This amount of energy is counted and stored. In achieving the specified Values, the device will trigger a signal through one or more contacts and / or make the desired switching. Through the Energy metered control will result in a uniform end product or uniformity by measuring the amounts of energy

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of the starting substances or their deviation with regard to the reaction behavior determine.

The mode of operation of this device is illustrated using the following example shown an exothermic reaction. This also applies analogously to an endothermic reaction.

If you want to check the uniformity of an isocyanate (Desmodur 44 V), proceed as follows: you take a known polyalcohol (test recipe 1 of the TAG), we want to call it the X component, and we want the isocyanate to be tested to be Y - Name the component and mix the X and Y components well according to the requirements (e.g. in the approximate stoichiometric composition). Now, a temperature sensor, e.g. a resistance thermometer, is placed in the center of the reaction vessel and measured This exothermic process, during the formation of a polyurethane coating, is the temperature. This temperature is converted, for example, according to Van ^N t Hoff's rule (10 temperature increase brings about a doubling of the reaction speed) into amounts of energy, with ExLfe a multiplication device and the like that, for example, the amount of energy at the start of the reaction is equal to 1 at 20 ° C. and 1 second. Then the converted amount of energy at 30 ° and 1 second is equal to 2, accordingly at 40 it equals 4 and at 50 it equals 8 etc ..

The counter now shows the amounts of energy occurring at each time unit count and save according to the temperature. The value 2 was found as the reaction coefficient for this example. For others Systems, other values are also possible. You have to set the factor in the multiplication device accordingly, so that again there is a growing series with regard to the assignment of temperatures.

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& 1LL IjU-J. bfci

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R = sum of the energy amounts counted or

the reaction units according to the energy expenditure

to = starting point time

te = end of reaction or termination of reaction R = reaction constant (in our case equal to 2) ω Τ = temperature difference

dt = differential coefficient of time

By choosing the components, the device can be put together in such a way that that at any desired temperature (according to the intended process) the starting point is 1. Instead of 1, you can also choose another suitable size. To simplify the measurement method you give the counter a certain maximum amount of energy, for this example 107 R, according to the desired conversion. is

Ji

if this is reached, the Time read off or automatically registered. If the energy consumption has now taken place in the same time as required, then the tested product is equivalent to. If there are deviations, the isocyanate to be tested does not react the same. It was found that the time tolerance 5 min. + 30 seconds, for a perfect batch of the Y component fraud. With this method you can quickly get the incoming Check goods and rate them at the same time. From the manual One is free to use the measuring method and its errors.

The present invention takes into account in the presence of different initial temperatures (independent of the device manipulated INPØ ⁴ P ^ start temperature) of the reactants through the progressive Bowertung the rising tone ^ oraturcr νηά preselected Posip- "r" f. ^v PP- ^; "-

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position on the counter a uniform end product. According to this principle other reaction partners of chemical processes can also be tested.

According to this example for the product investigation in the event of an exothermic Process, an example will now be given for the synthesis of a basic component in an endothermic process. Do you want to get out of one Dicarboxylic acid and dialcohol produce a polyester, so. if you choose 3 moles of polyalcohol and 2 moles of dicarboxylic acids, you get an ester ' with 4 ester groups and 2 terminal hydroxyl groups. The mixture is heated. The rate of esterification increases as the reaction temperature increases and thus the amount of water released as a measure of the progress of the reaction. The device according to the invention detected with the help of the temperature sensor and conversion into amounts of energy R the respective status of the esterification reaction and thus the amount of water released so far. The rate of distillation can now be determined from the newly acquired quantity of water control and regulate for optimal processes.

In the reaction vessel (still) in which the reactants are located a temperature sensor is installed.

The temperature is converted into reaction units R ₁ J as a function of time by the device according to the invention and displayed. These reaction units can be represented directly as the respective amount of water released by linking them according to the rules.

For the maintenance of the equilibrium the separation water and polyalcohol is necessary, the amount of water released ensures that the uniformity of the end product is maintained guaranteed.

No reactants required for the system are drawn off through incorrect distillation, only that which is undesirable for the end product Removed water.

Should be with one of the reactants for technical or chemical reasons are expediently worked with excess, so will

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cliow box dc ι. Wii.'JHui'iibiKihmc · iKM'iUikfjuihligl. DaK hoißl da.s Wasftor v / lrd constantly with a certain proportion of this reaction partner or this subtracted at the end of the process according to the programming. This gives you an equivalent end product regardless of the temperature profile and the batch quantities.

If you want to obtain a prescribed viscosity for the end product of a reaction that goes over 2 stages, with heat being supplied in one stage and heat being generated in the other stage, this device can be used to record the optimums of both stages by adding the individual reactants to Reaching predetermined number of pulses take place.

Instead of the Van ^v t Höfischen rule, one can also use the activation energy to help.

This then means a transformation according to

Re = / (η-Ί) Ln R _K dt « ΊΓ Γ Τα) οί /

R = reaction value in reaction units such as counter units of the present meter

R = reaction coefficient

T = temperature increase

A = activation energy

R = general gas constant

T (t) = time-dependent absolute temperature of the measuring point

t. t = start and end time of the process ο e ^ö

η = temperature-dependent exponent for

n-l = _J, η = 1 for T

10
T = start temperature of the reaction

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The examples given utilize the invention using the mathematical laws of natural growth or natural decline.

Such laws occur in chemistry, physics and biology. (Control of biological growth processes and proof of performance)

^{It was found that Van v} t Hoff's rule is sufficient for many processes, and that Arrenius' rule is more precise for others. These mathematical laws can be varied and adapted from case to case. Other relations are also applicable. The advantage of this method of energy measurement lies in the compensation of temperature fluctuations, since the corresponding amount of energy is assigned to each temperature interval and thus the conversion conditions of the reactants are taken into account. According to the conventional method, the processes must be run as a function of temperature and time. Now you can work under variable conditions and do not need to submit complicated programs. In the old programs, a failure of any kind of energy is never taken into account. The conversion now achieved can now be read from the energy equation at any point in time and, if necessary, the necessary measures for an equivalent production can be derived from it in the event of malfunctions.

A device suitable for this purpose of the invention consists of a resistance thermometer which is located in the measuring branch of a bridge circuit. The output voltage of the bridge is fed to a DC voltage amplifier supplied, added with a reference voltage and in an integrated amplifier with logarithmic wiring

after the function _, _ _π V ₁

2
V ₁ = input voltage

= k · R 1 transformed.

V ₀ = output voltage

C *

R = reaction constant depending on. Recipe in 0.1 steps

adjustable between 1, 6 and 2.5 k = 0.01 output voltage at input voltage 0

Another amplifier with an adjustable gain factor as evaluation drives the motor of a photoelectric type pulse generator.

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The Ixnpui «e; -; ind oms: un-dcii motor-applied voltage proportional. The impulses control an electromechanical one

Counter with preselection. After reaching the preselected number, an associated relay switches its contacts. A measurement trigger prevents the counter from counting if the temperature of the resistance thermometer is lower than the start temperature of the chemical reaction. The function equation is based on the display of the counter

No.

T ₁

- α J fl «

a = device constant, at T ₁ ζ. Β.

a = 1.28 pulses / min. J

Two examples of the construction of the device are then given using an electrical resistance thermometer and mechanical-optical analog-digital conversion (sheet 12, example 1) and using a thermocouple and electronic analog-digital conversion (sheet 12, example 2). ·

Circuit example 1 for the device is shown on sheet 12.

The resistance was thermometer component 1 applied to the measuring bridge component 2. Part 3 is a direct current amplifier. The logarithmic sound reinforcement according to U- = R ^. 1 takes place in component 4 for the logarithmic amplifier component 5.

A reduction device is used as a weighting factor for the meter housed in component 6.

Component 7 contains the power amplifier for the measuring motor in the component 8. Component 9 is a protective disk driven by the measuring motor and a photo-electric device for generating pulses Analog-to-digital converter.

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The mechanical pulse counter with preselection device and relay for the The output of signals is located in component 10. Component 11 is a signal lamp for remote display of the meter's operating status.

In example 2, module 12 represents the mains supply with constant holding for direct voltage, module 13 the device for temperature measurement with a thermocouple and DC amplifier. Module IS represents the logarithmic circuit for the output amplifier labeled with module 17 'according to the function U ₉ = R _x - 1. The electronic analog-digital conversion takes place in module 18, the pulse stretching in module 19 and the pulse shaping in module 20, The power amplifier in module 21 operates the mechanical pulse counter, module 22,

After module 13 is the connection of a directly indicating electrical Measuring instrument, module 25, intended for temperature reading .. In parallel with this, a measuring range subdivision, module 23 and a O-point control, module 24. The input of an external time signal. module 26 can be used to switch the counter. The counter 22 outputs a signal when certain pulse sums are reached intended. Module 27 is a constant equilibrium voltage source.

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Claims (1)

Pa t e η t a ns ρ r ü c h e '* Claim 1 ■. j ■ ^ / device for detecting, controlling or regulating the chemical j Reaction behavior and / or the amounts of energy used in chemical I. Processes or 'are released, and the laws of time Hr?. ~ J - visibly follow the reactances of the conversion, characterized in that! that the device has a sensor and a function circuit with: has a counter / which is running on a sample or Ee- ί reehnung determined reaction parameters can be set, and via the j the energy flow and / or the progress of the reaction detected, controlled. ■ | or is regulated. _f . - ■ [ tr i Claim 2 ■ ■ -. "- ■ · j Device according to claim 1, characterized in that ztir Control of the progress of the reaction via the function circuit -, .- ,. | or the counter is controlled by a programmer. ■ '· .- ■■ · ■: ■ ' Claim 3 Device according to claims 1 and 2, characterized in that the
Counter is provided with preselection and end-some intermediate contacts, so
that signals for the acquisition and control can be triggered. - Claim 4 Device according to claims 1, 2 and 3, characterized in that
the programmer for the automatic utilization of the 'from the "·
Function circuit or counter provides processed data. Claim 5 Device according to claim 1, characterized in that in the
Circuit function amplifier according to mathematical formulas from
Prepare data recorded by the sensor and, if necessary, preamplified for driving the counter and controlling the program. 10 9827/0653 BATH Claim 6 - ^v Apparatus according to claim 5, characterized in that the Puncture circuit drives a motor for analog-to-digital conversion. Claim 7 Device according to claim 6, characterized in that the motor to form the digital signal with a photoelectric pulse generator Possesses impulse stretching. Claim 8 Device according to claims 1, 3 and 6, characterized in that the input variable by the sensor with the help of a trigger suppression takes place as long as the input size falls below the desired start of work. Claim according to claims 1 and 8, characterized in that the Sensor a directly indicating measuring instrument with end and intermediate contacts operates without functional evaluation and without the suppression taking effect. Claim 9 according to claim S,. characterized in that the trip contacts of the direct-reading Measuring instrument to maintain the functional evaluation. Claim 10 according to claim 1,. characterized in that the sensor is an electrical thermometer is used. . Claim 11 according to Claim 1, characterized in that a radiation probe is used as the sensor. 109827/0653 BATH Blank page