DE3603971C1 - Method for operating a hot separator and associated device - Google Patents

Description

The invention relates to a method for operating one of the sump phase reactors of high pressure hydrogenation of coals, tars, mineral oils, their Distillation and extraction products and the like Substances downstream heat separator for which Separation of the mash from the bottom phase reactors into a bottom product, namely predominantly high-boiling Oils, ashes, possibly catalyst, undissolved coal and in volatile reaction products in the preamble of Claim 1 specified Art.

The invention further relates to a hot separator, from a pressure-resistant container, which is an upper one cylindrical and a lower conical wall insert contains and its content through a cooling system can be cooled by means of a cooling gas and the with nozzle for entry of the reacted products, Top product outlet, bottom product outlet, if necessary Hydrogenation gas inlet at the bottom of the conical insert, Level measurements and the cooling system is equipped.

It is known to avoid settling and Coking in the hot separators of the  High pressure hydrogenation of the inner walls for cooling indirectly through recycle gas To cool snake tubes to thereby Condensation and flushing on the inside wall of the To achieve separator (see. DE-PS 8 85 398).

Hot separators such as those used in systems for liquefying coal hydrogenation are used, consist of flameproof containers which Pipe coils contain cooled inserts to the To facilitate deposition and to prevent the hot separator wall, the separated ones, not coke volatile substances. The lower chilled Insert is usually designed as a funnel, through which the non-volatile components are removed will. Practical operation has shown that despite the effective cooling of the lower insert due to pipe coils often caused by coking disorders occur the irregular gait of the separator and even caused business interruptions (cf. DE-PS 9 71 419).

When hydrogenating coal, tars and heavy oils the reaction products from the Marsh phase reactors in a separator in order to Separation into a solid and predominantly high boiling oils existing solid / liquid phase and one the volatile reaction products as well Gases / vapors phase containing hydrogenation gas passed. To chemical after reactions, which too Polymerizations of the products and for the constipation of the  Separator may have to restrict the reaction products are cooled somewhat for this purpose, for example 10-40 ° C lower than that Temperature in the last sump phase reactors.

On the other hand, the reaction products in Separator at the highest possible temperature level be held to the thermal separation of the To carry out products in an energy-saving manner and, if necessary, around Waste heat from the reaction products to heat the To utilize products of the bottom phase hydrogenation.

In the known method for cooling the Inner walls in an indirect way through recycle gas the temperature of those in the separator Products lowered in that a cooling coil around the conical insert of the separator is wound, being between the inner and outer surface of the internals There is pressure equalization.

This coiled cooling coil has several Process engineering disadvantages: Between cooling coil and Form the outside of the conical insert the time solid deposits, which the Change the heat transfer coefficient. Hence can cause unwanted product Solid deposits on the inside of the conical use not by simple thermal measurements of the Thermal transmittance can be recognized. Furthermore, by means of a single cooling circuit  no optimal separate temperature setting of the in the conical use of the bottom product and the one in the cylindrical insert Gas / vapor phase possible.

Because of the different dwell times of the various products in the hot separator and different hydrogen supply - in the im conical insert located marsh product occurs there is increasing hydrogen depletion a need the temperatures of the in the conical Use of the bottom product and in the cylindrical gas / vapor phase to keep at predetermined levels to a chemical Post-reaction with polymerization and solid formation to prevent and still the highest possible Maintain temperature level in the hot separator.

This task is one method and one Device of the type specified above solved that the characteristics of the license plate of Claim 1 and claim 3 realized are.

Through precise thermal measurements of the Hot separator product temperatures, for example by means of attached to the inserts Thermocouples can be an undesirable training product-side coke and other Solid deposits on the cylindrical and the conical use can be effectively prevented.  

By manufacturing both the conical insert 4 and the cylindrical insert 3 from a spirally wound square hollow section 12 , by winding these inserts in circumferential turns, the cooling performance is improved overall.

The turns are on the inside of the sun inserts produced preferably by Welds joined together on the Are smoothed on the inside. On the outside of that Manufactured containers are the coils preferably by an interrupted outer load-bearing Seam joined together.

This structure leads to, preferably separate, integrated cooling circuits.

All turns of the conical insert 4, which is made of square profile 12 and form the conical insert 4, are welded to one another on the inside without interruption, the inner weld being the sealing seam and the outer seam being the supporting seam.

The windings of the cylindrical cooling coil from square profile 12 forming the cylindrical insert 3 are welded to one another on the inside in the same way as with the conical insert 4 without interruption, the inner weld seam being the sealing seam and the outer seam being the supporting seam.

The uppermost turns of the cylindrical cooling coil from the square profile 12 are expediently wound at a distance and are not welded to one another. They serve as expansion compensators during operation when heated.

The composite system consists of wound and welded square profiles 12 , preferably with a cylindrical bore, which simultaneously assume the functions of the cooling coil and the container wall.

Changes in the heat transfer coefficient - if the process conditions are otherwise the same - allow direct conclusions to be drawn about solid deposits on the inside of the heat separator 1 .

By means of the separate cooling circuits provided, the process-relevant temperatures of the bottom product located in the conical insert 4 and the gas / vapor phase located in the cylindrical insert 3 can be set independently of one another to the required values, and only hydrogen gas or hydrogenation gas is required to influence the Coking equilibrium in the hot separator, ie counteracting the hydrogen depletion occurring in the hot separator, the amount required, but not for the purpose of direct cooling of the hot separator contents, to be introduced directly into the hot separator.

In another embodiment of the proposed hot separator, it can be provided that the cooling circuits for the conical insert 6 and the cylindrical insert 5 are constructed from tubes 13 fastened to the inserts and welded to the respective insert.

The connection of the inserts 3 and 4 , or 5 and 6 can by a conical shot 11 z. B. be produced by means of a sheet metal element, so that a common apparatus element is present.

The proposed hot separator and in particular are the inserts through which the cooling medium flows suitable for an external pressure load of up to 700 bar and a temperature load of up to 500 ° C to withstand.

In Fig. 1, the construction of the proposed new hot separator 1 with the pressure-resistant container 2 and nozzle 7 for the entry of the reacted mash, top product outlet 8 and bottom product outlet 9 is shown schematically in a preferred embodiment. The conical insert 4 and the cylindrical insert 3 of the inner container each form an integrated, fixed composite system consisting of the cooling circuit and the container wall. Two separate coolant flows are applied to the conical and cylindrical inserts.

The coolant flows are for the conical insert 4 via sockets for cooling gas inlet ( 10/1 ) and cooling gas outlet ( 10/2 ), for the cylindrical insert 3 via sockets for cooling gas inlet ( 10/3 ) and cooling gas outlet ( 10/4 ).

The conical insert 4 has, for example, 10 degrees bevel and is wound from a square profile 12 with a cylindrical bore. The cylindrical insert 3 is also wound from the square profile 12 with a cylindrical bore, the connection of the two inserts being produced by the conical weft 11 , which can optionally be reinforced by ribs. The conical insert 4 is on the inside with, for example, four thermocouples 15.1, 15.2,. . ., 15 . N and the cylindrical insert 3 on the inside with, for example, two thermocouples 14.1,. . ., 14 . N equipped. The thermocouple connections can be led out of the hot separator 1 , for example, via gland seals.

The hot separator 1 is designed, for example, for a permissible operating temperature of 500 ° C. and a permissible operating pressure of up to 700 bar, with pressure equalization between the inside and outside surface of the internals.

According to another construction example shown in FIG. 2, cooling coils consisting of tubes 13 are wound around a thin cone wall 6 or cylinder wall 5 and welded on.

The reference numerals 1 and 2 again designate the hot separator and the pressure-resistant container. The reference numerals for the sockets 7, 8, 9, 10/1, 10/2, 10/3 and 10/4 and for the element 11 have the meanings given in the explanation of FIG. 1.

Here too there is pressure equalization between the inside and Outside surface of the cone or cylinder wall.

Claims (10)

1.Method for operating a hot separator downstream of the sump phase reactors of high-pressure hydrogenation of coal, tars, mineral oils, their distillation and extraction products and similar substances, for the separation of the reacted products from the sump phase reactors into a sump product, namely predominantly high-boiling oils, ash, if necessary Catalyst, undissolved coal and in volatile reaction products, constructed from a pressure-resistant container which contains an upper cylindrical and a lower conical wall insert and the contents of which can be cooled by a cooling system by means of a cooling gas, characterized in that the temperatures of the in the conical insert sump product and the gas / vapor phase in the cylindrical insert are kept by means of integrated cooling circuits for indirect cooling at the values which may be required to limit chemical after-reactions in the hot separator, and may differ. 2. The method according to claim 1, characterized in that that by thermal measurements undesirable formation of product-side coke and other solid deposits on the inside cylindrical and conical insert is registered. 3. Hot separator, constructed from a pressure-resistant Container with nozzle for entry of the reacted Products, head product exit, Bottom product outlet, possibly hydrogenation gas entry on Bottom of the conical insert, level measurements and Cooling system, characterized in that integrated cooling circuits with nozzles for Cooling gas inlet and outlet for the conical Use as well as with connection for cooling gas inlet and -Outlet intended for cylindrical use are. 4. Hot separator according to claim 3, characterized characterized that both the conical use as well as the cylindrical insert with Thermocouple connections for measuring the Hot separator product temperatures and the Measuring lines from the pressure chamber of the hot separator are brought out. 5. Hot separator according to claim 3, characterized characterized that the integrated Cooling circuits for the conical and the cylindrical insert made from a spiral  wound square hollow profiles Verbund system exist. 6. Hot separator according to claim 3, characterized characterized in that the conical and the cylindrical insert made of a square hollow section with a cylindrical bore in circumferential Turns are wound. 7. Hot separator according to claim 6, characterized characterized in that the turns on the Inside with weld seams connected, these welds on the inside smoothed out and that the turns on the outside due to an interrupted outer load-bearing seam are interconnected. 8. Hot separator according to claim 3, characterized characterized in that the cooling circuits for the conical and the cylindrical insert made on tubes attached to the inserts attached to the are welded to the respective insert are. 9. Hot separator according to claim 3, characterized characterized in that the two inserts by a Sheet metal element to a common apparatus element are put together. 10. Hot separator according to claim 3, characterized characterized by the cooling medium  flowed through inserts of an outer Pressure load of up to 700 bar and one Withstand temperatures up to 500 ° C.