JPS5828656A - Measuring apparatus of differential heat, differential pressure and viscosity at the same time - Google Patents

Abstract

PURPOSE:To perform a reaction analysis while carrying three kinds of measurements at the same time by providing sample room and standard room independently having pressure measuring apparatus and themocouple and measuring the differential pressure and differential heat between rooms and providing a sensor for viscosity measurement in the sample room, in addition. CONSTITUTION:In case of a catalyst activity test, for instance, under high pressure hydrogenation decomposition of coal paste, the coal, a catalyst and hydrogen, are taken in a standard room 19 without stirring and a sample 9 composed of the coal and compounding oil, the catalyst and hydrogen, are taken in a sample room 7 and then, both rooms are set up in one electric heating furnace 12. The room 7 is provided with a rotary resistance plate for viscosity measurement 8, a rotary shaft for stirring resistance measurement 6, a torque measuring sensor 5 and a slip ring for torque meter 4 to measure the viscosity, while stirring at the same time and the viscocity is measured. Each differential heat measuring sensor 10, 11 and differential pressure measuring sensors 16, 16, are provided in the rooms 7 and 19. Output of the sensors 10, 11 is sent to a differential heat output amplifier 20 and that of the sensors 16, 16 is sent to a differential pressure output amplifier 15. The amplifiers 20, 15 and a torque sensor output amplifier 14, are connected with a recorder 18.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an apparatus for simultaneously measuring differential heat, differential pressure and viscosity.

Conventionally, differential heat measurement has been used as a means of measuring the physical properties of natural or synthetic organic or inorganic compounds in order to elucidate their phenomena. It is said (゛Special public Akibatake s -
gssso issue). Differential thermal measurement employs a method in which the temperature 'i' of a sample and a sample is raised or lowered at a constant rate to determine the temperature difference caused by heat absorption or heat generation at the 'transformation point' of the sample. As mentioned above, differential thermal measurement requires heating the sample at the same speed as one chamber, and at the differential heating temperature of a chemical reaction, it is necessary to stir the sample in order to control the temperature. In any case, heating is applied from the outside, so if the physical properties of the substance change by 1 degree, for example, the viscosity changes, the stirring will change, and the heat conduction within the sample will become uneven, causing the apparent A differential thermal curve based on a typical chemical reaction cannot be obtained. In addition, by stirring strongly, changes in heat conduction due to changes in viscosity can be ignored (if this is done, the heat generated by the mechanical energy caused by stirring will be transferred to the sample, making it impossible to measure differential heat). , when analyzing a chemical reaction using a differential heat line, it is impossible to accurately analyze a chemical reaction unless the temperature-viscosity curve during summer is measured and analyzed simultaneously with the measurement of the differential heat. Become.

For example, when testing the catalytic activity by measuring the differential heat of high-pressure hydrogenolysis of coal paste, the temperature of the coal paste made of coal (II blue coal) and blended oil is measured. S・or 5oot
When the temperature reaches 5 sots, the bituminous coal swells and dissolves in the blended oil, resulting in a very high viscosity, and when the temperature reaches 5 sots, the viscosity becomes low. When the viscosity is high, the stirring of the coal paste becomes insufficient and a uniform differential heat curve cannot be obtained. Therefore, when measuring the differential thermal curve during high-pressure hydrocracking of coal paste, if the high-pressure hydrogenation reaction is carried out with coal, catalyst, and hydrogen without using blended oil, and without stirring (reference sample ) and compare it with the differential heat curve of a case (sample) in which a coal paste consisting of coal, a catalyst, and a blended oil is reacted with hydrogen under stirring. It is not possible to analyze the effects of blended oil on coal, catalyst activity, etc.

The present invention provides an independent sealed sample chamber and a reference chamber for filling a sample or reference sample and a gas that reacts with the sample, and each chamber is connected to a barometric pressure measuring device to measure the differential pressure between each chamber. In addition, each chamber is equipped with a thermocouple to measure the water difference between the sample chamber and the reference chamber, and the sample chamber is equipped with a senna shaft for viscosity measurement that does not touch the inner wall surface. Measuring senna (with resistor plate)
The viscosity of the sample is applied to the viscosity measurement sensor by rotating the sample chamber or by rotating the sample chamber itself with a constant torque.The viscosity of the sample is measured by simultaneously measuring the viscosity of the sample by measuring the viscosity of the sample. It is related to the device.

Below, the apparatus of the present invention will be described as No. 19! Let me explain with one IK.

The sample volume and reference chamber 19 are placed inside an electric heating furnace designed to heat the inner 11 surfaces at a constant rate and in a beautiful manner.
Inside the sample w17 is a viscosity measuring rotary resistance plate (Masatsu resistance plate) 8 for measuring the viscosity of the sample and stirring at the same time, and a stirring resistance measuring device rotating shaft 6 connected thereto. A torque measuring sensor S and a torque meter slip ring 4 are provided to measure viscosity, and an internal rotating permanent magnet 8 and an external rotating permanent magnet for rotating the rotating shaft 6! Also, a constant rotation speed is provided. A silk measuring sensor power supply 13 and a torque measuring sensor output amplifier 14 are connected to the torque meter slip ring 4 . Also, sample chamber 7
and the reference chamber l$ are each equipped with a differential thermal measurement sample sensor 10.
Differential thermal measurement standard part sen'? 11 and a differential heat output amplifier 20 are provided to measure the threshold differential heat between chambers 7 and 19. Each chamber 7 and 19 measures the change in internal pressure, so each chamber has a differential pressure measurement sensor 1 and a differential positive output amplification @
It is linked to Is. In addition, each chamber is provided with one valve for feeding the reaction gas, and a differential thermal output amplifier 11115, a differential positive output amplifier 11115, and a lux measurement sensor output amplifier 914 are each equipped with water. It was connected to a differential hot water differential pressure viscosity recorder 18, so that differential heat differential pressure viscosity could be measured simultaneously.

Another example of the device of the present invention is shown in the accompanying drawings.

Instead of stirring the sample as intended, the sample chamber itself can be rotated.

In such a case, the rotating shaft 6 (numbers in the figure are the same as in FIG. 1) does not rotate, but is merely an axis that transmits changes in silk due to changes in sample viscosity.

Using the apparatus of the present invention, the differential thermal differential pressure and viscosity were simultaneously measured using a sample of coal-based mixture of bituminous coal and blended oil (anthracene oil) (4:6), and using coal alone as a reference sample. The results are shown in Figure 8. The measurement conditions were as follows: A fixed amount of the sample and a reference sample were placed in a sample chamber and a reference chamber, respectively, and the chambers were filled with 100% hydrogen at the start of the measurement, and the temperature was raised from room temperature to SOO ℃ at a rate of 2 ℃ per minute. When the temperature reaches 450℃, the hydrogen pressure is about 200℃.
% has been reached. The temperature difference and pressure difference between the sample chamber F and the reference chamber II at each temperature when this temperature was maintained for one hour were measured. At the same time, the viscosity of the coal paste in the sample chamber was measured.

The apparatus of the present invention is for analyzing a three-phase reaction such as a direct liquefaction reaction of coal, such as a body, a liquid, and a gaseous body, and can be used for performance tests of catalysts for coal liquefaction reactions.

That is, when examining the activity of a catalyst, when differential heat during temperature rise appears simultaneously with differential pressure, it can be considered that the reaction heat is due to hydrogen absorption. In addition, if there is no change in the differential pressure (or a change only in the differential heat), it can be considered that the solid phase coal has absorbed the blended oil and swelled, or that the coal has dissolved in the blended oil. When studying these phenomena, it is possible to judge whether the coal belongs to the blended oil or whether it has dissolved in the blended oil based on the temperature-viscosity curve measured at the same time.This allows for a detailed analysis of the high-pressure hydrocracking of coal. .

[Brief explanation of the drawing]

FIG. 1 of the accompanying drawings is a detailed explanatory diagram of the present invention. The second drawing is a partial explanatory diagram of another apparatus of the present invention, and FIG. 8 is a diagram showing a simultaneous measurement curve of differential hot water differential pressure viscosity in a coal high-pressure hydrogenation reaction measured by the apparatus of the present invention. In FIGS. 1 and 3. 1--Constant rotation motor. 2--An externally rotating permanent magnet. Hatake-ichi internally rotating permanent magnet. 4--) Slip ring for rutameter. 5-1 Silk measurement senna. 6-- Rotation shaft for measuring stirring resistance in the sample. 7--Sample room. $--Viscosity measurement rotating resistance plate. To sample 10 - Differential thermal measurement sample part Senna. 11-Differential heat measurement reference section Senna. 1 - 1 electric heating furnace. 11--) Router measurement sensor power supply. n=-Silter measurement sensor output amplifier. 1! - Increased differential pressure output. t@- differential pressure output measurement sensor. 1? --Gas inlet valve 18--Differential thermal differential pressure viscometer. 19--1 Single room. 20-Differential thermal power multiplier. 21-Mechanism for converting one rotating part into a fixed part. 22-1 Viscometer sensor fixing part 385

Claims (1)

[Claims] Separate and sealed sample chambers and reference chambers are provided to collect the sample or reference sample and the gas that reacts with the sample, and each chamber is connected to a barometric pressure measuring device to measure the differential pressure between each chamber. In addition, a thermocouple was installed in each chamber to measure the same differential heat between the sample chamber and the reference chamber, and a senna for viscosity measurement was installed in the sample chamber so that it did not come into contact with the interior of the chamber. A simultaneous differential pressure and viscosity measurement device for differential hot water, characterized in that it measures the viscosity of a slope. □