Multi-feeding and reaction integrated device and method for microcalorimeter
A technology of multiple feeding and microcalorimetry, applied in feeding devices, chemical instruments and methods, mixers with rotating stirring devices, etc., can solve the problems of main reaction ratio reduction, instrument damage, ratio increase, etc. Achieve the effect of avoiding over-range, expanding application range and reducing risk
Active Publication Date: 2018-01-23
XIAN MODERN CHEM RES INST
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Problems solved by technology
In these two test processes, only one feed can be realized. For the strong exothermic test process (such as nitration reaction, sulfonation reaction, etc.) or the process of side reactions, the test process will have the following problems: (1) due to the material It is added at one time, and there will be severe exothermic heat during the reaction process, and the whole test is not easy to control, which will cause the instrument to exceed the range (such as attached figure 1 As shown), there is even a risk of damaging the instrument; (2) If there are side reactions in the reaction process, one-time feeding will cause the material to be at the maximum concentration at the beginning of the reaction, so that the proportion of side reactions will increase, and the proportion of main reactions will increase. decrease, and the measured calorific value deviates too far from the real value, which cannot faithfully reflect the actual heat of the process
Method used
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Embodiment 1
[0027] The nitration reaction of malononitrile is taken as an example for specific illustration.
[0028] At 20°C, add 5mL of mass fraction of 5% acetic acid aqueous solution and 0.325g of malononitrile in the reaction tank of the sample cell, and evenly place a total mass of 0.69g of sodium nitrite on the 8-layer discharge platform. Add 5 mL of 5% acetic acid aqueous solution and 0.325 g of malononitrile into the reaction tank of the reference pool, assemble and seal the reaction devices of the sample pool and the reference pool respectively. After the microcalorimeter reaches the reaction temperature, put the whole device into the microcalorimeter, start the motor, and after the heat flow of the system is stable, adjust the height of the feeding paddle according to the scale line on the upper surface of the stirring rod so that it reaches the first layer first Rotate the vertical stripes 2-3 times to ensure that the materials on the discharge table are completely added to th...
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The invention discloses a multi-feeding and reaction integrated device and method for a microcalorimeter, which aims to solve the problem that when the existing microcalorimeter conducts a semi-batch reaction test, it can only realize one-time feeding but cannot perform multiple feedings, resulting in over-range or even Problems that damage the instrument. The device can place the materials to be fed on the discharge tables of different heights. When feeding, adjust the height of the feeding paddles to make them reach the discharge tables of different heights in turn, and rotate to make the materials enter the reaction tank in batches to achieve multiple The purpose of secondary feeding. The multi-feeding method for the microcalorimeter disclosed by the invention includes five steps. The invention can be used in the semi-batch reaction test of the microcalorimeter, so that the reaction can be fed multiple times, avoiding the problem of over-range in the test process, reducing the risk of the test process, and expanding the application range of the microcalorimeter.
Description
technical field [0001] The invention belongs to the field of physical and chemical testing, and mainly relates to a multi-feeding and reaction integrated device and method for a microcalorimeter in the reaction heat testing process. Background technique [0002] A semi-batch reaction is one in which at least one reactant is added while the reaction is in progress. Compared with the batch reaction, the semi-batch reaction mainly has two advantages: (1) for the exothermic reaction, the exothermic rate can be controlled by adding materials, so that the reaction exotherm is within a controllable range; (2) if the reaction process There are side reactions, and the gradual addition of the reaction materials helps to maintain the concentration at a low level, which helps to improve the reaction yield. Therefore, the study of semi-batch reaction has more important safety and economic significance. [0003] Among research methods, microcalorimeters have higher calorimetric efficien...
Claims
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IPC IPC(8): B01J19/18B01J19/00B01J4/00B01F7/18G01N25/20
CPCB01J4/001B01J19/0093B01J19/18G01N25/20B01F27/90
Inventor 祝艳龙丁黎安静梁忆周静
Owner XIAN MODERN CHEM RES INST