DE1032217B - Process and device for the decomposition of liquid and solid reaction products - Google Patents

Description

It is customary to remove reaction products which contain liquid and solid substances, optionally in a solvent or diluent, by filtration to disassemble and then work up the solid and the filtrate separately. In continuous operation however, difficulties arise when the solid has a large surface area, voluminous is dispersed in solvents and is very difficult to wash out. In this In case one has to accept larger solvent losses. Also contain the reaction products easily polymerizable or unstable compounds, the use of thin-film or falling-film evaporators also helps in the work-up not a satisfactory solution.

Ordinary steam distillation fails in such cases, e.g. B. in the processing of the Reaction product of the cyclooctatetraene synthesis. if only because the deposition of resinous Nel> en products that like niprene on the walls of the Vessels lead to encrustations and smears, making continuous distillation impossible.

It has now been found that with such solid-liquid mixtures, especially those that Contain unstable compounds that break down into solid and liquid parts under gentle conditions succeeds if one enters a water column a little below the surface d: there is water water vapor initiates in such a way that a swirling steam-water zane arises above the surface of the liquid and in this introduces the mixture, the liquid fractions being evaporated, while the solid fractions • Sink down through the eddy-free water column below the steam supply and are discharged will.

This procedure has the advantage that the volatile, liquid fractions of the to be evaporated Evaporate and distill the mixture immediately after being in with the steam for a very short time Touch were. A polymerization of easily reacting parts of the mixture, as in the usual Steam distillation, especially in the presence of catalysts, occurs frequently thereby avoided. A particular advantage of working is that the solid parts of the Reaction product through the water column below the supply of water vapor, which has a calming effect represents supply zone, sink immediately down and can be removed continuously. they are not, as is often the case with separation by ordinary steam distillation, ζ. B. at the Decomposition of Products of Cyclooctatetraensynihese is the case, greasy, but of a powdery nature. Since the water column is below the Method and device

for breaking down liquids and solids

Reaction products

Applicant:

Aniline & Soda Factory in Baden

Aktiengesellschaft,

Ludwigshafen / Rhine

Dr. Walter Reppe, Heidelberg,
Dr. Karl Baur and Dr. Walter Schweter,

Ludwigshafen / Rhine,
have been named as inventors

Steam supply is eddy-free, the solid fractions are not deposited on the wall and onto it Wise encrustations, which would make an interruption of the distillation process necessary, avoided. Due to the special arrangement of the immersion of the distillation vessel, the solid components sink through the open, conical bottom into the second container.

When carrying out the process, the water vapor is, for example, 4 atmospheres below the Introduced into the water surface, so that a swirling steam-water zone is formed above it or to which the mixture to be worked up is introduced from above. In this zone the liquid Fractions evaporated by the water vapor and discharged together with it. The vapor mixture will condensed in a cooler and the condensate in the separating vessel in an aqueous and organic layer separated. The organic layer is then broken down, e.g. B. by distillation into their components. In order to avoid losses, the aqueous layer, since it mostly contains organic components, is dissolved contains, expediently in the Distillationsvorrich led back. If the boiling point of the organic components dissolved in the water is higher than 100 ° C, so you can evaporate the overflowing water and use again as steam for distilling. The salts dissolved in the water, e.g. B. un-

809 557/401

Catalysts needed can be recovered using the usual methods.

The process can also be carried out under reduced pressure. You have to get one accordingly apply deep water diving, d. that is, the hydrostatic pressure of the water column in this case must be the Pressure drop correspond to the atmosphere.

The drawing shows an example of a device for carrying out the method. In a bottom conically tapered boiler 1, which is provided at the top with an overflow 2, at the bottom with a spacious lock 3 and filled with water up to the level of the overflow, there is a second container 4. This is with its lower, open, also the conical part is immersed in the filled kettle 1 in such a way that the water reaches the tapered point of the container. The steam supply 5 takes place through a ring line 9 which is provided with bores at the top. It is installed in such a way that the steam is blown upwards 10 to 30 cm below the surface of the water. The cylindrical part of the container 4, which protrudes from the immersion and is determined as a vapor space, has sight glasses 5 ″ at the height of the water level. A vapor pipe 6 leads from the vapor space to the cooler 7, from which the condensate drains into a separating vessel 8. The mixture to be broken down is pumped in through the elbow connector 10 approximately halfway up the vapor space. The nozzles 11 and 12 are used to rinse the sight glasses 5 a, including in the

In this case, water draining from the separator is used.

Claims (2)

PATENT CLAIMS: 1. Process for the decomposition of mixtures containing liquid and solid substances, in particular those which contain unstable compounds, with steam, possibly under reduced Pressure, characterized in that a little below the surface of the water column Water introduces water vapor in such a way that a swirling vapor-water zone above the surface of the liquid arises and introduces the mixture to be separated into this, the liquid components are evaporated, while the solid fractions through the eddy-free water column below the Steam supply drop down and are discharged. 2. Apparatus for performing the method according to claim 1, consisting of a bottom conically tapered boiler (1), the one at the top with an overflow (2), at the bottom with a spacious one Lock (3) provided and filled with water up to the level of the overflow and into the one second, open at the bottom and conically tapered boiler (4) is immersed, its vapor space with a cooler (7) and separation vessel (8) is connected. 1 sheet of drawings © 809 557/401 6.58