Method for cleaning water-saturated flow, received during fischer-tropsch reaction

FIELD: method for separating at least a fraction of non-acidic chemical products from at least a fraction of raw gaseous product received in Fischer-Tropsch reaction, or from condensate of said product.

SUBSTANCE: in accordance to method at least a fraction of raw gaseous product or its condensate is fed into feeding plate of distillation column, liquid flow is drained from aforementioned column from plate, positioned above feeding plate of the column. Received liquid flow is divided on water phase and saturated non-acidic chemical product phase and water phase is returned to distillation column onto plate positioned below plate from which liquid flow is drained.

EFFECT: increased efficiency of cleaning method.

23 cl, 1 dwg

 

The technical field

The present invention relates to an improved method of separating non-acidic chemical products from enriched water stream produced in the reaction of the Fischer-Tropsch (FT).

Rationale inventions

In the following description, the term "NK" means non-acidic chemical products selected from the group comprising acetone and higher ketones, methanol, ethanol, propanol and higher alcohols, i.e. oxygen-containing hydrocarbons, with the exception of acids.

The term "hydrocarbon" means a hydrocarbon, usually insoluble in water, such as, for example, paraffins and olefins.

Enriched water stream produced in the plant for carrying out the Fischer-Tropsch synthesis (FT), contains a variety of oxygenated compounds such as alcohols, aldehydes, ketones, carboxylic acids and similar substances that are products of synthetic reaction FT. These compounds are (partially) in the water flow due to their partial or complete solubility in water.

To remove non-acidic chemical products (NCH), such as alcohols, ketones, aldehydes and other non-acidic compounds of the enriched water flow requires the use of distillation columns to the water of improved quality can be processed next, and then return to the environment. Enriched NK stream from the distillation column can be processed further in order to obtain certain products or it can be found an alternative use.

Division NCH and water fraction in distillation columns, usually called a column for the distillation of the reaction water (column PDFs), is complicated by the extremely non-ideal properties of water and heavy organic fraction present in the water flow, especially With4and heavier alcohols. This imperfection facilitates the Stripping of these compounds from enriched water liquid phase below the feed plate, which is the purpose of the specified column. However, above the feed plate, as the water content in the liquid inside the column is reduced, heavier alcohols are less volatile and have a tendency to re-condense.

The heavy alcohols begin to accumulate in the column, eventually forming a second liquid phase. This oxygen-containing hydrocarbon phase contains much more heavy alcohols and much less water than the first phase. If the second liquid phase leaving the column, it will create a path to the low volatility to heavy alcohols migrated down until they again pass into the vapor state under the action of rising through the column of vapor. This leads to the circulation of oxygen-containing hydrocarbons, such as, for example, heavy alcohols, inside the column to poor distribution of the liquid on the plates and, finally, to skip the heavy material in the bottom of the column. This breakthrough will cause the formation of the cubic product that does not meet its specifications, and will cause problems in the equipment for water treatment, located downstream, due to the dirt.

Thus, oxygen-containing hydrocarbon phase formed inside the column, usually removed with a relatively small steam flow in the lower part of the column, usually of a few plates above reboiler. This steam stream is then condensed and separated into two phases. Enriched water stream is then sent to the column, or mixing it with the boot material, or directing it to the column separately. Oxygen-containing hydrocarbon phase is usually mixed with the main stream for further processing.

However, this exhaust steam is insufficient for such a complete removal of oxygen-containing hydrocarbon phase, so that it no longer appeared in the column. The steaming allows you to remove just as much oxygen-containing hydrocarbon phase to slow breakthrough in CBM product. Thus, in the column is extensive circulation of the organic phase, which makes the column relatively ineffective for separating chemicals from the water.

Brief description of the invention

The present invention provides a method of separating at least F. the shares of non-acidic chemical products (NCH) from at least fractions of crude gaseous product, obtained in the reaction of the Fischer-Tropsch (FT), or from condensation of the specified product, comprising at least the steps:

supply at least fractions of crude gaseous product or condensate to the feed plate distillation columns;

- selection of the liquid flow from the specified column from the plate located above the supply tray;

- separation of the liquid flow in the aqueous phase and enriched NK phase; and

- the return of the aqueous phase in the distillation column on a plate below the plate, with which the selected liquid stream.

The method may include removing hydrocarbons range C5-C20of condensate crude gaseous product during the preliminary operation.

Pre-operation may include the condensation of the gaseous raw product and then split it into three-phase separator. Three threads coming out of the separator can be: tail gas, hydrocarbon condensate, mainly comprising hydrocarbons range From5-C20and the so-called stream of the reaction water containing NK, water, acid and suspended hydrocarbons.

The flow of the reaction water may, for example, have the following composition (mass.): 96% water, 3% NCH, approximately 1% acid and from about 0.05 to 1% suspended hydrocarbons range From5-C20 .

Suspended hydrocarbons can then be separated from the flow of the reaction water by any suitable separator capable of separating a stream on a suspension of hydrocarbons and enriched water stream.

Applied by the separator may be an oil coagulant, usually Pall coagulator capable of removing hydrocarbons from the stream of the reaction of water to achieve a concentration of 10 parts per million to 1000 parts per million, usually 50 parts per million.

The coagulator is designed to increase the size of the droplets suspended hydrocarbons that were easy to implement separation type liquid - liquid.

If the hydrocarbons contained in the flow of the reaction water (usually from 0.05 to 1 wt.%.), not removed before the start of distillation, they can cause foaming inside the distillation column or can contaminate CBM product, resulting in this product will not meet the requirements of the specification requirements for hydrocarbon content.

In an alternative embodiment of the separator or coagulator established not before distillation column, and use it instead to separate the hydrocarbons from the cubic product distillation columns of the distillation residue.

The separated hydrocarbons may be filed by recycling to the operation of three-phase separation or directed in the installation for which abode hydrocarbons, below the stream.

Enriched water stream obtained by removing suspended hydrocarbons, is fed into the distillation column. Enriched water stream may contain some amount of carried out free of oil remaining after coagulation, and from 1 to 10 wt.% NCH.

Distillation column used for the implementation of this method can have from 30 to 60, usually from 38 to 44 of the plates.

The supply plate distillation columns may be located between 7 and 15 plates, and this is usually the plate 10 (the numbering of the plates from the top of the column down).

The liquid stream can be withdrawn from the column with a plate located directly under the plate on which first appears or is produced enriched NK phase, and this plate is located above the feed plate, thus hindering the movement of the specified phase in the lower region of the column and subsequent recycling in the upper part of the column. Then, the liquid stream may be separated into an aqueous phase and a phase enriched NK.

The liquid stream can be withdrawn from distillation column with plates, located between the plate 4 and the plate 13, usually a plate 6 (the numbering of the plates from the top of the column). The liquid stream may be separated into an aqueous phase and a phase enriched NK, with the help of decanter, positioned and what about the inside or outside of the column.

The aqueous phase is returned to the column on the plate, below the plates, with which the selected liquid flow, typically, this plate is located directly under the plate, with which the selected liquid stream.

Separated phase enriched NK, can be mixed with the main products of the distillation column for further processing, or it can be processed independently to highlight your own valuable components, or it can be served in a setting for a hydraulic control treatment (IPF hydrroprocessing unit), which is usually in the same place as the distillation column.

Enriched NK phase obtained in the separation of a liquid stream taken from the column may contain from 90 to 100%, usually 95 wt.%. NCH (mainly including heavy alcohols), while the aqueous phase may contain from 80 to 100%, usually about 94 wt.% water.

Depleted NK and enriched water stream can be extracted in the form of the cubic product of the column.

VAT product mainly include water and organic acid-rich water flow, as well as the minimum number NCH, usually about 50 parts per million. Before further processing or before discharge into the environment CBM product can be used for heating the enriched water stream flowing in the distillation column

The stream enriched NK and containing water, can be extracted in the form of the head product of the column.

The mode of operation of the column may be such that the head product contained from 15 to 45%, typically from 25 to 30 wt.% water.

Detailed description of the invention

The invention will be further described in the following non-limiting example with reference to the attached drawing, which shows a diagram of an embodiment of a method in accordance with the present invention.

In the drawing, the number 10 position usually indicates a way of separating at least a fraction of non-acidic chemical products (NCH) from 28 fractions enriched in condensed water, raw gaseous product 12 produced in the reaction 14 Fischer-Tropsch (FT).

The method 10 includes a preliminary operation in which the suspended hydrocarbons are removed from the fractions of crude gaseous product 12.

Preliminary operation includes the condensation of the gaseous raw product 12 and separating it in a typical three-phase separator 16. The separator 16 leave three streams: the tail gas 18, hydrocarbon condensate 20, mainly comprising hydrocarbons range From5-C20and the so-called thread 22 of the reaction water containing NK, water, acid and suspended hydrocarbons.

Thread 22 of the reaction water typically has the following composition (wt.): 96% water, 3% NCH, p is blithedale 1% acid and from about 0.05 to 1% suspended hydrocarbons range From 5-C20.

Thread 22 of the reaction water is then separated using Pall coagulator 24, which divides the stream 22 of the reaction water, the suspension 26 hydrocarbons and enriched water stream 28.

Pall coagulator 24 is capable of removing hydrocarbons from the stream 22 of the reaction of water to achieve a concentration of 10 parts per million to 1000 parts per million, usually 50 parts per million.

Suspension 26 hydrocarbons or served by recycling in a three-phase separator 16 or send in installations for the processing of hydrocarbons (not shown)located below in the course of the stream.

Then enriched water stream 28 serves to distillation column 30 on the supply plate 32.

The liquid stream 34 is withdrawn from the column with 30 plates located above the feed plate 32. The liquid stream 34 includes two liquid phases formed in the distillation column 30, namely a phase enriched NK, and enriched with water or aqueous phase. The selection of the liquid stream 34 essentially means removing almost all the liquid from the column 30, the result at this stage of the column 30 is removed greatest possible number of enriched NK phase.

Then the liquid stream 34 is separated into the aqueous phase 36 and phase 38, enriched NK, after which the aqueous phase 36 returned to distillation column 30 on the plate, below the plates, with which the selected liquid flow any NCH and enriched water stream 40 is extracted in the form of the cubic product of the column 30. Enriched NK stream 42 containing water, remove the top (head) of the product of the column 30.

Distillation column 30, as shown in figure 1, has 42 plates. The feeding plate 32 is a plate 10 (the numbering of the plates from the top of the column 30 down), and a liquid stream 34 is extracted from the plate 6 (the numbering of the plates from the top of the column 30). In the shown embodiment the liquid stream 34 is separated by the decanter 44 located outside the column 30. The mode of operation of the column 30 is usually that the lead product 42 contains from 15 to 45%, typically from 25 to 30 wt.% water. CBM 40 product contains mainly water and organic acids from a crude product 12, and the minimum number NCH, usually about 50 parts per million. Enriched NK stream 38 typically contains 95 wt.% NCH (including mainly heavy alcohols), while the aqueous phase 36 typically contains approximately 94 wt.% water. Before further processing or before discharge into the environment CBM product 40 is used for heating the enriched water stream 28 coming into the distillation column 30, through heat exchanger 46.

The following table presents the experimental data obtained by the separation of the enriched water stream having a composition similar to the composition, usually defined in enriched water flows from the installation is of the Fischer-Tropsch synthesis, in accordance with the operations described above method, starting from the moment when enriched water stream 28 serves to distillation column 30.

Table
Composition, wt.%Enriched water stream 28Head product 42Enriched NK phase 38CBM product 40
Water98,126,28,399,8
Aldehydes<0,1<0,10,00,0
Ketones<0,10,50,10,0
Methanol and ethanol1,353,03,30,0
Alcohols, C3, C4 and C50,519,527,80,0
Alcohols C6+<0,10,445,90,0
Other NKh<0,10,39,0<0,1
Acid0,10,2the 5.70,1
Flow (kg/h)703,6 21,70,6682,5

The results clearly show that enriched NK phase, which was previously accumulated above the feed plate, essentially removed from the column via stream 34 of the liquid and ultimately is recovered in the form of enriched NK phase 38. Significant destruction of enriched NK phase, thus preventing the accumulation of heavy alcohols in the column, which in turn eliminates the problems associated with this accumulation, as described above, and enables efficient separation of NK from enriched water stream 28.

It should be understood that the present invention is not limited to any specific embodiment or configuration, is described and illustrated in this document.

1. Method of separating at least a fraction of non-acidic chemical products (NCH) from at least fractions of crude gaseous product obtained in the reaction of the Fischer-Tropsch (FT), or from condensation of the specified product, including at least the following operations:

feeding at least a fraction of crude gaseous product or condensate on the supply plate distillation columns;

the selection of the liquid stream from the specified column from the plate located above the supply tray;

the separation of the liquid flow in the aqueous phase and enriched the th NCH phase and

return the aqueous phase in the distillation column on a plate below the plate, with which the selected liquid stream.

2. The method according to claim 1, wherein the method includes removing hydrocarbons range C5-C20of condensate crude gaseous product at the preliminary operations.

3. The method according to claim 2, in which the method includes a preliminary operation, which includes the condensation of the gaseous raw product before separating it into three-phase separator.

4. The method according to claim 3, in which three threads coming out of the separator is the tail gas, hydrocarbon condensate, comprising mainly hydrocarbons range C5-C20and the flow of the reaction water containing NK, water, acid and suspended hydrocarbons.

5. The method according to claim 4, in which the suspended hydrocarbons are then separated from the flow of the reaction water by any suitable separator capable of separating a stream on a suspension of hydrocarbons and enriched water stream.

6. The method according to claim 5, in which the applied separator - oil coagulator.

7. The method according to claim 6, in which the flocculating agent is capable of removing hydrocarbons from the stream of the reaction of water to achieve a concentration of 10 parts per million to 1000 parts per million.

8. The method according to claim 1, in which a two-phase separator and/or a flocculating agent applies the Ute for separating hydrocarbons from the cubic product distillation columns.

9. The method according to claim 5, in which the separated hydrocarbons are served by recycling into the separator.

10. The method according to claim 5, in which the enriched water stream is served in the distillation column.

11. The method according to claim 1 in which the distillation column is from 30 to 60 plates.

12. The method according to claim 1 in which the distillation column is from 38 to 44 of the plates.

13. The method according to claim 1, in which the supply plate distillation column is between the plate 7 and the plate 15 when the numbering of the plates from the top of the column down.

14. The method according to claim 1, in which the supply plate distillation column is a plate 10.

15. The method according to claim 1, in which a liquid stream is withdrawn from the column with a plate located directly under the plate on which first appears or is produced enriched NK phase.

16. The method according to item 15, in which the liquid stream is then separated into an aqueous phase and a phase enriched NK.

17. The method according to clause 16, in which the liquid stream is separated into an aqueous phase and a phase enriched NK through the decanter, located inside or outside the column.

18. The method according to claim 1, in which a liquid stream is withdrawn from the distillation column with plates, located between the plate 4 and the plate 13.

19. The method according to claim 1, in which the liquid stream is taken from the plate 6 distillation columns.

20. The method according to claim 1 in which the aqueous phase is returned to the column on the plate, the location is percent lower plates, with which the selected liquid stream.

21. The method according to claim 1 in which the aqueous phase is returned to the column on a plate located directly under the plate, with which the selected liquid stream.

22. The method according to claim 1, in which the operation mode of the column is such that the head product contains from 15 to 45 wt.% water.

23. The method according to claim 1, in which the operation mode of the column is such that the head product contains from 25 to 30 wt.% water.



 

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FIELD: catalyst preparation methods.

SUBSTANCE: invention provides Fischer-Tropsch catalyst, which consists essentially of cobalt oxide deposited on inert carrier essentially composed of alumina, said cobalt oxide being consisted essentially of crystals with average particle size between 20 and 80 Å. Catalyst preparation procedure comprises following stages: (i) preparing alumina-supported intermediate compound having general formula I: [Co2+1-xAl+3x(OH)2]x+[An-x/n]·mH2O (I), wherein x ranges from 0.2 to 0.4, preferably from 0.25 to 0.35; A represents anion; x/n number of anions required to neutralize positive charge; and m ranges from 0 to 6 and preferably is equal to 4; (ii) calcining intermediate compound I to form crystalline cobalt oxide. Invention also described a Fischer-Tropsch process for production of paraffin hydrocarbons in presence of above-defined catalyst.

EFFECT: optimized catalyst composition.

16 cl, 12 tbl, 2 ex

FIELD: petroleum chemistry, chemical technology.

SUBSTANCE: method involves carrying out the preparing synthesis gas by the gaseous oxidative conversion of natural gas with air oxygen, catalytic conversion of synthesis gas to a catalyzate followed by its cooling and separating and feeding a liquid phase into reactor for synthesis of gasoline. For aim reducing the cost of manufacturing catalytic preparing methanol is carried out in the synthesis reactor wherein methanol is fed into reactor for preparing high-octane components of gasoline that are stabilized and separated for liquid components and fatty gas that is fed into reactor for preparing oligomer-gasoline. Then liquid components from reactors wherein high-octane components of gasoline and oligomer-gasoline are prepared and then combined, and the mixture is stabilized. Water formed in all synthesis reactions after separating is removed separately, combined and fed to the fresh water preparing block and formed nitrogen is fed for storage with partial using in technological cycle and in storage of synthetic fuel. The unreacted depleted synthesis gas from block wherein methanol is prepared is used for feeding methanol into reactor sprayers for preparing high-octane component of gasoline, and unreacted gases from reactor for preparing oligomer-gasoline are fed into generator for synthesis gas. Also, invention claims the device for realization of the method. The device consists of blocks for preparing synthesis gas, catalytic conversion of synthesis gas to catalyzate and preparing gasoline and made of two separate reactors for preparing high-octane additive of gasoline and oligomer-gasoline. The device is fitted additionally by block for preparing fresh water and nitrogen collector. The reactor sprayers are connected with intermediate capacity for collection of methanol and with reactor for synthesis of methanol and block for preparing methanol, and reactor for preparing oligomer-gasoline is connected pneumatically with block for preparing synthesis gas. Invention provides the development of method for the combined preparing the fuel and fresh water.

EFFECT: improved preparing method.

2 cl, 6 dwg, 2 ex

FIELD: petrochemical process catalysts.

SUBSTANCE: preparation of crusted metallic catalyst comprises: (i) applying suspension containing diluent, catalytically active metal selected from cobalt and ruthenium groups, and optionally first refractory element (atomic number at least 20) oxide onto surface of carrier particles to form wet coating and (ii) removing at least part of diluent from wet coating, said suspension containing at least 5% by weight of catalytically active metal based on the weight of calcination residue, which would result after drying and calcination of suspension. Crusted metallic catalyst itself and hydrocarbon production process are also described.

EFFECT: simplified catalyst preparation technology, improved physicochemical properties of catalyst as well as selectivity thereof, and increased productivity of hydrocarbon production process.

10 cl, 1 tbl, 3 ex

FIELD: municipal services; devices for decontamination of the running water.

SUBSTANCE: the invention is pertaining to the devices for decontamination of the running water with the varying in time its turbidity and containing in its composition predominantly the hardly- oxidizable substances, pathogenic bacteria, viruses and may be used for treatment of the water consumed for the household activity and drinking needs, for decontamination of the biologically purified waste waters at their pouring out in the reservoir and for other similar purposes. The device for decontamination of the running water contains: the ultra-violet emitter, the reflector, the source of the industrial oxygen, the ozonizer, the jet device, the spiral vane, the upright-tubular system, the concentration meter of the dissolved ozone in the running water, the setting device, the comparator, the tracking drive, the gate unit, the reverse valve, the cock, the electrified shutters, two pressure detectors and the control unit. At that the device additionally contains the turbidity meter, the functional transformer and the switchboard. At that the mixing chamber of the jet device is made out of the quartz glass, the ultra-violet emitter consists of the separate ultra-violet lamps arranged axially in respect to the quartz mixing chamber of the jet device, the turbidity meter is mounted at the inlet of the jet device, the outlet of the turbidity meter is connected to the inlet of the functional transformer, the control unit is connected to the outlet of the functional transformer and with the inlet of the switchboard and the outlet of the switchboard is connected to lamps of the ultra-violet emitter. The technical result of the invention consists in the increased efficiency of decontamination of the running water at its turbidity varying in the time.

EFFECT: the invention ensures the increased efficiency of decontamination of the running water at its turbidity varying in the time.

2 dwg

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