JPS62185785A - High temperature separation method and separator - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a 'i+ 77n'r The raw material for the liquid phase reactor is converted into liquid phase product 1■J in a classifier with a high NJl content.
It relates to a method for separating point oil, ash, optionally catalyst, insoluble coal and volatile reaction products.

Furthermore, the present invention provides a pressure-tight container comprising an upper cylindrical insert and a lower conical insert, the contents of which are cooled by means of a cold power J device through which a cooling gas is passed, and a connection for the inflow of reaction products. Tube piece, connection piece for the outflow of the head product, connection piece for the outflow of the liquid phase product, connection piece for the inflow of the hydrogenation gas, possibly at the bottom of the conical insert, liquid level measuring device. and a high temperature separator consisting of a pressure vessel with a cooling device.

[Conventional technology]

In order to avoid deposits and carbonization in high-temperature separators for high-pressure hydrogenation, it is known to perform a condensation action and flushing on the inner walls of the separator by indirectly cooling the inner walls by circulating gas through coiled tubes (Federal Republic of Germany). Patent No. 88539
No. 8 specification 1Ki).

High-temperature dividers, such as those used in coal liquefied hydrogen addition bags (tit), are used to facilitate separation and to prevent separated non-volatile materials from carbonizing on the hot divider walls. It consists of a pressure vessel containing an insert that is cooled by a coiled tube.The lower insert that is cooled is usually configured as a hopper, through which the non-volatile components are discharged.As a result of practical operation, the coiled tube It has been found that, despite effective cooling of the lower insert by carbonization, frequent failures occur due to carbonization, leading to irregular operation of the separator and even to interruptions in operation (German Patent No. 97).
+419 details).

During the hydrogenation of coal, tar and n(oil), the reaction products of the liquid phase reactor are a solid-liquid phase consisting of solids and mainly high-boiling oil, and a gas containing volatile reaction products and hydrogenation gas. - the reaction products are cooled slightly to limit re-reactions which could polymerize the products and clog the separator, e.g. It must be cooled to 10-40'C below the temperature inside the reactor.

On the other hand, the reaction products in the branching vessel are kept at the highest possible temperature level, so that the thermal branching of the products can be carried out in an energy-saving way, and in some cases the waste heat of the reaction products can be transferred to the charge product for liquid-phase hydrogenation. Used for heating.

In the known method of indirectly cooling the inner wall with circulating gas,
Wrap a cold J-coil around the conical insert of the separator;
By balancing the pressure between the inner and outer surfaces of the insert, the temperature of the product within the insert is reduced.

This wound cooling coil has numerous drawbacks. Initially, solid deposits form over time between the cooling coil and the outer surface of the conical insert, changing the heat transfer coefficient. Undesirable product-side solid deposits occurring inside the conical insert therefore cannot be confirmed by simple measurements of the heat transfer coefficient. Furthermore, a single cooling circuit does not allow separate optimum temperature setting of the liquid phase product in the conical insert and the gas-vapor phase in the cylindrical insert.

[Problem that the invention seeks to solve]

Due to the different residence times of the individual products and the different amounts of hydrogen supplied (the liquid phase product inside the conical insert becomes progressively depleted of hydrogen), the liquid phase product inside the conical insert It is necessary to maintain the temperature and the temperature of the gas-vapor phase within the cylindrical insert at a predetermined value to maintain as high a temperature level as possible in the high-temperature separator while preventing re-reactions with polymerization and solid formation. .

[Means for solving problems]

For this purpose, according to the method of the invention, the temperature of the liquid phase product in the conical insert and the γ of the gas-vapor phase in the cylindrical insert are reduced. +;! g and integrated cooling power 1 for indirect cooling.
A circuit holds the temperature at the value necessary to limit re-reaction within the high temperature reactor. To carry out this method, the high-temperature separator has an integrated cooling gas inflow and outflow connection piece for the conical insert and a cooling gas inflow and outflow connection for the cylindrical insert. A cooling circuit is provided.

The undesirable formation of coke and other solid deposits at cylindrical and conical inserts can be prevented by accurately measuring the temperature of the hot separator product, for example using thermoelectric elements provided in the inserts. It can be effectively prevented.

By making conical and cylindrical inserts from helically wound hollow square profiles and winding these inserts as annular turns, the overall cooling capacity can be improved.

The windings are connected to each other preferably by welded seams on the inside of the insert thus produced, and these welded seams are smoothed on the inside. On the outside of the container thus produced, the windings are preferably connected to one another by means of intermittent support seams. This structure provides preferably separate and integrated cooling circuits.

All turns of the coil forming the conical insert from hollow square profiles are welded together without interruption on the inside, the inner weld seam serving as a sealing seam and the outer weld seam as a support seam.

The turns of the cooling coil forming the cylindrical insert from the hollow square profile are welded together without interruption on the inside, similar to the conical insert, the inner weld seam as a sealing seam and the outer seam as a supporting seam. It is valid.

The top turns of the cylindrical insert of hollow square profiles are preferably wound at intervals and not welded together. This winding serves as an expansion compensator when the temperature increases during operation.

The composite system consists of hollow square profiles with preferably cylindrical holes and rolled and welded, these hollow square profiles taking over the functions of the cooling coil and the vessel wall.

Changes in the heat transfer coefficient, other things being equal, lead directly to the presence of product side solid deposits inside the high temperature separator.

Separate cooling circuits allow the temperature of the liquid phase product in the conical insert and the temperature of the gas-vapor phase in the cylindrical insert to be set to the required values independently of each other, and the hydrogen gas or hydrogenation gas , necessary to influence the carbonization equilibrium in the high-temperature external vessel, that is, necessary to resist the hydrogen depletion that occurs in the high-temperature external vessel [1 t, but the high-temperature external Nu t? H contents [! It is not intended to be directly cooled, but it is sufficient to directly transfer it to the high-temperature separator.

In other configurations of high-temperature sliding, the cooling circuit for the conical insert and the cooling circuit for the cylindrical insert can be formed from tubes that are attached by welding to the respective inserts.

The two inserts can be connected, for example, by a conical piece made of a metal plate to form a common device element.

The proposed high-l crystal separator, especially the insert passed through a cold 1JJfS body, is suitable for external pressures up to 700 bar and 500' (:
Suitable to withstand temperatures up to.

〔Example〕

FIG. 1 shows a new high-temperature separator with a pressure-resistant vessel 2, a connection piece 7 for the inflow of the reacted feedstock, a connection piece 8 for the outflow of the head product, and a connection piece 9 for the outflow of the liquid phase product. The structure of l is shown schematically. The conical insert 4 and the cylindrical insert 3 of the inner container form an integrated fixed system of cooling circuit and container wall. The conical insert and the cylindrical insert are supplied with two separate coolant streams.

The cooling medium flow for the conical insert 4 is routed through the connecting tube piece 10/I for cooling gas inflow and the connecting tube piece 10/2 for cooling gas outflow, and the cooling medium flow for the cylindrical insert 3 is routed through the cooling gas inlet connecting tube piece 10/I and the cooling gas outlet connecting tube piece 10/2. Connecting tube piece 10/3 for cooling gas outlet and connecting tube piece 10/4 for cooling gas outflow
After that, you will be asked.

The conical insert 4 has an inclination angle of, for example, lOo and is wound from a hollow square profile 12 with a cylindrical hole. The cylindrical insert 3 is likewise wound from a hollow rectangular profile 12 with a cylindrical hole, and the connection between the two inserts is carried out by a conical piece 11, which can optionally be reinforced with fins. The conical insert 4 has, for example, four thermal lightning elements 15 on the inside.
I, 15.2...15. N, the cylindrical insert 3 is equipped with, for example, two thermoelectric elements 14.1 . ...+4
-N is provided. The terminals of the thermoelectric element can be drawn out from the hot portion @","41 via, for example, a gasket.

For example, the high temperature separator l has a permissible operation of 500'C R+i and 7
It is designed for a permissible positive operating pressure of up to 00 bar, with pressure equalization between the inner and outer surfaces of the insert.

According to another construction example shown in FIG. 2, a cooling coil consisting of a tube I3 is wound around a thin conical wall 6 and a cylinder 5 and welded. Reference numbers l and 2 again indicate the high temperature separator and the pressure vessel.

Connecting tube piece 7.8.9.10/I, 10/2.10/3
．． The symbols 10/4 and conical piece 11 have the meanings given in the description of FIG.

In this case too, a pressure equilibrium takes place between the inner and outer surfaces of the conical wall and the circle aVt.

[Brief explanation of drawings]

FIG. 1 is a longitudinal cross-sectional view of a first embodiment of a high temperature separator according to the present invention, and FIGS. 1X and 1Y are W portions of the
1 and 2 are longitudinal sectional views of the second embodiment, and FIG. 2X is an enlarged view of the X portion thereof. l...+:'5'j7i'1 atomizer, 2...pressure vessel, 3...cylindrical insert, 4...conical insert, 7...for reaction product inflow Connection pipe piece, 8... Connection pipe piece for head product outflow, 9... Connection pipe piece for liquid phase product outflow, 10/I, 10/3... Connection pipe piece for cooling gas inflow, 10/2, IO/4... Connecting pipe piece for cold 13 gas outflow, 12... Hollow rectangular shaped material.

Claims (1)

[Claims] 1. An upper cylindrical insert and a lower conical insert connected after a liquid-phase reactor for high-pressure hydrogenation of coal, tar, mineral oil, their distillation and extraction products, and similar substances. The reaction product of the liquid phase reactor is separated into liquid phase products, mainly high-boiling oil, ash,
In some cases, in the process of separating catalyst, insoluble coal and volatile reaction products, the temperature of the liquid phase product in the conical insert and the temperature of the gas-vapor phase in the cylindrical insert is A high-temperature separation process characterized by an integrated cooling circuit for indirect cooling to maintain the values necessary to limit re-reaction in the high-temperature separator. 2. Process according to claim 1, characterized in that temperature measurements record the undesired formation of product-side coke and other solid deposits inside the cylindrical and conical inserts. . 3 Connection piece for the inflow of the reaction products, connection piece for the outflow of the head product, connection piece for the outflow of the liquid phase product, and optionally the connection piece for the hydrogenation gas at the bottom of the conical insert. Consisting of a pressure-tight container with an inlet connection piece, a liquid level measuring device and a cooling device, a connection piece for the inflow and outflow of cooling gas for the conical insert and a connection tube for the inflow and outflow of the cooling gas for the cylindrical insert. High-temperature separator, characterized in that it is provided with an integrated cooling circuit having an integrated cooling circuit. 4. Claim No. 4, characterized in that the conical insert and the cylindrical insert have a thermoelectric element for measuring the hot separator product temperature, the measuring line leading out of the pressure space of the hot separator. High temperature separator according to item 3. 5. Claim 3, characterized in that the integrated cooling circuit for the conical insert and the cylindrical insert consists of a composite system made up of hollow square profiles wound in a spiral manner. High temperature separator as described in. 6. High-temperature separation according to claim 3, characterized in that the conical insert and the cylindrical insert are wound in an annular winding from a hollow rectangular profile with a cylindrical hole. vessel. 7. Patent claim 7, characterized in that the turns are connected to each other on the inside by welded seams, these welded seams on the inside are smoothed, and the turns are connected to each other on the outside by intermittent supporting seams. A high temperature separator according to scope 6. 8. High-temperature separation according to claim 3, characterized in that the cooling circuit for the conical insert and the cylindrical insert consists of a tube attached to the respective insert by welding. vessel. 9. High-temperature separator according to claim 3, characterized in that both inserts are combined into a common device element by a metal plate. 10. High-temperature separator according to claim 3, characterized in that the insert through which the cooling medium is passed is resistant to external pressures of up to 700 bar and temperatures of up to 500°C.