DD267570A1 - METHOD FOR CHARACTERIZING THE REACTION BEHAVIOR OF CARBON AND COAL PROCESSING PRODUCTS - Google Patents

Abstract

The invention relates to a method for characterizing the reaction behavior of coal and coal processing products, with the aid of reaction processes, z. For example, the formation of new phases, extraction processes and aging processes can be quantitatively quantified and dynamically monitored in the material system solid - liquid. Thus u. a. in the systems coal or coal processing products - fluid statements on the carbochemical performance behavior of coal are made. The basis for the process are density changes occurring in solid-liquid reactions, which are directly related to the immersion weigh-time-time curves to be measured. The hydrostatic operation is realized in a prepared analytical balance. The sample container is a pycnometer.

Description

For this 2 pages drawings

Field of application of the invention

The invention relates to a measuring method, with the aid of reaction courses, z. B. phase regeneration, extraction processes and Arterungsvorgänge in the material system solid-liquid quantified and can be viewed dynamically. The basis for this are the density changes occurring in such systems in defined reactions, which are directly related to the measurable changes in the immersion weight value.

Characterization of the state of science and technology

Significantly .linde information for the chemical upgrading of coal provides statements on the extraction behavior with various solvents. Here, not only the previously used quantitative extraction yields of interest, but also more accurate knowledge of the temporal course of the reaction, the .undsätzlich express in a Qu ° and a 'can be divided feaktionsprozeß.

No direct method is known, according to which statements can be made quickly and simply concerning the course of the processes with regard to temporal quantification of the extractive treatment of coals. However, the temporal reaction dependence of the extractions is practical, since this interaction for dynamic carbochemical processing Ver''en, z. Ti. In the catalytic high-pressure Hyrter, can be pulled.

Furthermore, for Kohleveredlutigsprozesse in which the coals can not be processed dusty and a mashing process is necessary, a characterization of the mashing behavior of the coal, in particular the aging behavior under elevated temperatures (T <160 ⁰ C) before. special interest.

A disadvantage of the previously described and sufficient methods is that bo! The extraction of coals so far only total quantitative statements can be made that do not allow a reference to the temporal course of reaction interesting.

A routine method for determining the aging behavior of Kohlemai is not known. In the absence of these methods, it is not possible to make any tentative statements on the change in the mashing behavior, although the interactions between coal and McFcitch may actually have a significant influence on the actual coal upgrading process. Significant wire a slight characterization of the reaction courses between liquids and coal or carbon sequential products, which can be detected even in temperature ranges outside normal temperature.

The invention aims to provide a method for the rapid and accurate characterization of the Reaktionsvorgänrja between coal, coal products and liquids especially in their timely forerun. An elucidation of the chemical changes should be easily determined from studies on the temporal course of the reaction. Since routine operations in factory laboratories require a simple and fast method with easy-to-implement material technical conditions, there is a real need for a corresponding method.

Explanation of the essence of the invention

The invention has for its object to detect the lateral Reaktionsveriauf between coal and coal products on the one hand and liquids on the other hand quantitatively. It was recognized and scientifically justified that the inclusion of an immersion weighing-time-curve can make a contribution to the solution of the task. Immersion Weigh Value means the apparent weight of the sample in contact with a liquid. This value corresponds to the difference between weight and hydrostatic buoyancy.

Running In a defined system, which is in equilibrium with both forces, reactions take place in such a way that a change in the density of the solid takes place in the solid by incorporation of liquid molecules or extraction of solid substances, this results in a change in the immersion weight value. If this value increases in the coal-liquid system, this fact can be explained by a phase regeneration. This allows the quantitative Erfar treatment per unit time and volume of the solid used newly formed phases.

The stated object is achieved according to the invention by determining the immersion weight value of a vessel which has a capillary opening and a further opening for introducing solid matter, such as a pycnometer or the like. The vessel is dried and filled with solid. The liquid is introduced and intimately mixed with the solid, z. B. in the ultrasonic bath. The filled vessel is attached to a weighing device and immersed in a reservoir with the same amount of liquid until it is completely below the surface. Now the immersion weight value of the filled vessel m Iv ₉ ) is determined and the time to notated. At time intervals not exceeding half an hour, the immersion weight value of the filled vessel mi (t) is read and the measured values are correlated with each other. One bears Ami / mi against t, where

Yank _d With)-

mi mi (to) - mn

and m _{tl is} the immersion weight value of the liquid filled but no sample containing pycnometer at the same temperature. A mathematical evaluation of the recorded value pairs, z. Eg by means of an iterative regression for a function of the type

Ami => At _m ", i (1 - exp - -) ⁿ

where Ami - change of Immersionswägev.artes

At _1n U ₁ I - maximum value of Arrii after completion of the reaction

t - time

τ, η - parameters

are possible.

The evaluation of the determined by measuring points and mathematically defined curves allows statements to

following aspects:

1. Reaction Revenue - The Iterative Value Determined On _mw , i allows predictions about the expected

Reaction conversion or the content of soluble or cleavable components.

2. Reaction type - difference in shape of the value of the parameters allows for statements about

Qualities / suitability of various coals, coal products or liquids

3. Reaction speed - The detection of the reaction rate allows the optimization of technological

Parameters, e.g. B. Determination of an optimal mashing temperature. The invention will be explained in more detail below using an exemplary embodiment. AusfChrungsbeispiel The figure illustrates the experimental setup. Test procedure:

1. Fill the pycnometer with the test material (about half full, always the same amount of felling).

2. Fill up the liquid so that the sample quantity is covered (note down ZeW).

3. Mixing in an ultrasonic bath. The pycnometer is immersed in the bath only up to the neck, in order to avoid that bath liquid gets into the pycnometer.

4. Continue to fill in pycnometer liquid and stopper with ground capillary with as little loss of internal liquid as possible.

5. Attachment to the scale whose zero point has been previously set.

6. Recording the change in the immersion weight value as a function of time.

7. After completing the 6th Immersion Weighing of the empty pycnometer.

8. Formation of the relative immersion value change Anv'mi, where rri | (t _o ) is the first measured value of immovable weighing.

9. Graphical representation of the value pairs (t; Ami / m,) and / or mathematical-statistical processing.

Thus, the proposed measurement method for solids or mixtures of solids, which tend to involve the formation of new phases with the involvement of liquids, can quantify these new growths dynamically. This also applies to extractive reactions, eg. As to coal and coal products. The larger Ami / rtii, the greater the extraction potential of the investigated coal.

experimental measurements

As an example, two carbon powders were investigated. The immersion liquid used was tetrahydrofuran, which is one of the extractants used in practice. Other possible immersion liquids are:

a) for extractive studies solvents and chemicals such as toluene, ethanol, pyridine and the like;

(b) for mash assays, cabbage-derived low, medium and heavy oils, petroleum oils and model mash fluids such as tetialin, 1-methyl-naphthalene, etc., alone or in admixture.

The immersion curves are shown in the diagram:

- sample of EGR dust (electro filtered coal undersize from the briquette factory Bohlen)

- Sample yellow coal from the Delitzsch South / West mine.

The coal with the greater extraction potential is the yellow coal from the Delitzsch South / West mine.

Claims (8)

1. Antecedents for characterizing the reaction behavior of coal and coal products which are in a solid state and which show a density change on contact with liquids by introducing Fiüssigkeitsmolekülen or by extraction of solid, characterized in that the Immersionswägewert a filled with test material and liquid vessel , which contains an opening for introducing solid and liquid, which is closable with its stopper or the like, which has a capillary opening, is determined at defined time intervals and the immersion weighing value change is correlated to the passage of time. 2. The method according to claim 1, characterized in that a dry vessel such as a pycnometer o. Like. Is filled with solid to be examined, liquid is introduced, solid and liquid are intimately mixed, the vessel is closed in such a way that only through the capillary mass exchange with the environment is possible, the filled vessel attached to a weighing device and in a container is completely submerged with the liquid, the first immersion weighing value is determined, further values are determined in time intervals of 1 to 30 minutes and the relative immersion weight change Δπΐ | / ιτΐ | is correlated to t. 3. The method according to claim 1 and 2, characterized in that the liquid is an organic solvent such as toluene, ethanol, pyridine o. The like. 4. The method according to claim 1 and 2, characterized in that the liquid is light, medium, heavy oil, tetralin, 1-methylnaphthalene o. The like. 5. The method according to claim 1 and 2, characterized in that the solid represents carbon particles or powder. 6. The method according to claim 1 to 5, characterized in that the mixing takes place by means of ultrasound. 7. Verfahron according to claim 1 to 6, characterized in that the time interval of the Immersionswägewertmessung is 30: nin 8. The method according to claim 1 to 7, characterized in that the mass transfer with the environment via the filling opening of the vessel takes place.