Method of removing methylacetylene/propadiene (mapd) from hydrocarbon streams (options)


C10G70/02 - by hydrogenation

 

Usage: petrochemistry. Essence: conduct selective hydrogenation of methylacetylene and PROPADIENE (MAPD) enriched in propylene stream. selective hydrogenation is conducted stepwise in the first single-pass reactor with a fixed bed , and then in a distillation column reactor containing a catalyst for hydrogenation supported on a carrier PdO, which serves as a component of a system for distillation. Effect: increase the conversion and selectivity to propylene. 2 N. and 12 C.p. f-crystals, 1 tab., 3 Il.

The technical field,

The invention relates to the removal MAPD from hydrocarbon streams. More specifically, the present invention relates to a method in which MAPD turn into valuable propylene by selective hydrogenation. More specifically, the invention relates to a method, in which one of the hydrogenation reactor is a distillation column, in which propylene is simultaneously separated from the stream containing unreacted MAPD.

Prior art

Methylacetylene/PROPADIENE (MAPD) is not a compound, and includes unstable compounds methylacetylene and PROPADIENE that may be pictured as Ob propylene stream. The simplest method of removal is selective hydrogenation, which not only removes the pollutants and turn them into a valuable product propylene. Then the flow of propylene is subjected to distillation to remove part of the stream, which contains not turned MAPD. A stream containing not turned MAPD, called “green oil”, and distillation column used to separate stream containing not turned MAPD, from propylene called “column-green oil”.

In the methods of the prior art for the selective hydrogenation MAPD in the flow of propylene was used as the liquid-phase and vapor-phase reactors. Usually, although the conversion is good, in both cases, over time, the selectivity decreases rapidly. Therefore, it would be desirable to improve the selectivity in General and save selectivity over time. As in vapor-phase and liquid-phase system using at least two reactors in parallel, sometimes three, leaving at least one free for regeneration.

The main disadvantage of this method is that the selectivity for propylene is not always as we would like. A byproduct of hydrogenation, however, is propane, which is not STV produced valuable propylene.

The concept of “reactive distillation” is used to describe simultaneously flowing in the column reaction and separation into fractions. For the purposes of the present invention the definition of “catalytic distillation” includes reactive distillation and any other process that is running at the same time reaction and fractional distillation in a column regardless of the destination.

The preferred catalytic distillation is a distillation, in which distillation is also used as catalyst of the reaction. Using the solid catalyst in the form of particles as part of the system for distillation in combination with a distillation column reactor for the various reactions described in U.S. patent No.(etherification) 4232177; (hydration) 4982022; (dissociation) 4447668; (aromatic alkylation) 5019669 and (hydrogenation) 5877363. In addition, U.S. patent No. 4302356, 4443559, 5431890 and 5730843 describe the catalytic system, which can be useful as systems for distillation.

Hydrogenation is a reaction of hydrogen with multiple carbon-carbon bond with the formation of saturated compounds. This reaction is known for a long time and it is usually performed at pressures above atmospheric, and at moderate temperatures, using bolactia hydrogenation, are platinum, rhenium, cobalt, molybdenum, Nickel, tungsten and palladium. Usually in the industrial forms of catalyst used, the oxides of such metals on the carrier. The oxides are reduced to the active form, or to use with a reducing agent, or in the process of applying the hydrogen in the raw material. These metals also catalyze other reactions, with the most noticeable dehydration at elevated temperatures. In addition, with increasing residence time in the reaction zone they can contribute to the reaction of olefinic compounds themselves or other olefins to form dimers or oligomers.

Selective hydrogenation of hydrocarbon compounds known for quite some time. Peterson and co-authors in the publication “The Selective Hydrogenation of Pyrolysis Gasoline”, presented to the Petroleum Division of the American Chemical Society (September 1962), discuss the selective hydrogenation of C4and higher diolefins. Boitiaux with co-authors in the publication “Newest Hydrogenation Catalyst, Hydrocarbon Processing, March 1985, are General, non-binding overview of the various applications of hydrogenation catalysts, including selective hydrogenation enriched in propylene flow and other factions. Normal Jidkova pressure of hydrogen, usually over 200 pounds/square inch and more often in the range of up to 400 pounds/square inch or more. Liquid-phase hydrogenation of the partial pressure of hydrogen is essentially the pressure in the system.

In the description of the patent UK 835689 disclosed hydrogenation With2and C3fractions at high pressure in a jet flow of liquid in order to remove acetylenes. Selective hydrogenation MAPD in the propylene streams using only catalytic distillation is discussed in international publication WO 95/15934.

The advantage of this method is that PROPADIENE and methylacetylene, located in the hydrocarbon stream in contact with the catalyst selectively converted into propylene with very little education, if any are formed, oligomers, or small, if it happens, saturation monoolefins contained in raw materials.

The invention

The present invention includes the selective hydrogenation of methylacetylene and PROPADIENE (MAPD) contained in enriched propylene stream, in order to clear the stream and producing large amounts of propylene. In a class of preferred embodiments of the invention is enriched in propylene stream is fed together with hydrogen vacilando-reactor and in contact with the hydrogen in the reaction zone, containing a hydrogenation catalyst such as supported on a carrier oxide of palladium, preferably in the form of a catalytic system for the distillation. The hydrogenation catalyst in a single-pass reactor with a porous layer may be the same catalyst or a catalyst, other than the column-reactor catalytic distillation. Hydrogen is supplied as needed to maintain the reaction and is believed to restore oxide and save it in a state of hydride. Distillation column reactor operates at such pressure that the reaction mixture boils in the catalyst bed. If desirable, the lower nedohin containing more high-boiling materials (green oil), can be shown to achieve complete separation.

Monotremes(s) of the reactor(s) with a fixed layer may(may) be any(s) of the reactor(s), the renowned(e) in this area, which is(e) may(may) contain a hydrogenation catalyst.

The rate of hydrogen should be adjusted so that it was enough to keep hydrogenation reactions and recovery loss of hydrogen from the catalyst, but it should be kept lower than that required for the hydrogenation of propylene, and in the case of the catalytic reactor, peo hydrogen” as used here. Usually the molar ratio of hydrogen to methylacetylene and PROPADIENE in raw materials in the fixed layer will be approximately from 1.05 to 2.5, preferably from 1.4 to 2.0.

In some embodiments of the invention may be described as comprising the following stages:

(a) feeding (1) a first stream containing propylene, methylacetylene and PROPADIENE and (2) a second stream containing hydrogen, in a single-pass reactor with fixed bed, where part of methylacetylene and PROPADIENE reacts with hydrogen with the formation of propylene;

(b) flow coming from the stage (a), in a distillation column reactor in the area of raw materials;

(c) simultaneously in the specified distillation column reactor (i) contacting the unreacted methylacetylene and PROPADIENE with hydrogen in the reaction zone of the distillation with a hydrogenation catalyst capable of acting as a system for distillation, resulting reacts more part of the specified methylacetylene and PROPADIENE with the specified hydrogen with the formation of additional quantities of propylene; and

(ii) the Department contained propylene by fractional distillation; and

(d) removing the separated propylene together with any quantity of propane and more Les is on stream. Optionally the method includes removing any quantities With4or more high-boiling compounds from the specified distillation column reactor in the form of lower nedogona. Hydrogenation when there is practically no loss of propylene.

Brief description of drawings

In Fig.1 in schematic form a flow diagram of one embodiment of the invention.

In Fig.2 in schematic form a flow diagram of a second variant embodiment of the invention.

In Fig.3 in schematic form a flow diagram of a third variant embodiment of the invention.

Detailed description of the invention

The raw material for the present method can usually be lower ndogoni from deethanizer installation for the production of ethylene. However, any threads that contain propylene contaminated MAPD, may be candidates for use in this process. In a specific embodiment of the invention a conventional single-pass reactors, fixed bed, preferably steam, to increase the conversion and selectivity together with a distillation column reactor instead of a column of green oil. The benefits of using a distillation column reactor instead of a column green is 2.5 odds, resulting in increased plant capacity. When the catalytic distillation of the hydrogenation the hydrogen is used more efficiently, thereby providing savings in current spending. Characteristic features of the distillation reactor type, such as limited time of contact of the product with the catalyst and the washing effect of the internal phlegmy, lead to less accumulation of carbon on the catalyst and longer intervals for the reaction between regenerations for additional savings in current spending.

2. The frequency of regeneration is reduced due to the exclusion of the second layer.

3. Convert columns of green oil for catalytic distillation-hydrogenation is simple and can be done during regular maintenance. The impact on the work of installation is minimal while the potential simplifying installation by eliminating the reactor.

4. Freed of the reaction vessels can be used for other purposes.

The catalyst that is acceptable for this process, contains 0.05-5 wt.% PdO on extruded aluminum oxide, for example, 0.3 wt.% PdO 1/8" extrudates Al2O3(aluminum oxide), catalytic hydrogenation, provided U is proizvoditeli, below.

This catalyst can be used, or in a single-pass reactors or distillation column reactor (column green oil). However, so that it can be used in a distillation column reactor, it must be so shaped that, at the same time, to perform the function of the system for distillation, which for some distillation columns may be a simple catalyst loading. There are several methods and systems available to more good works, which are described in U.S. patents№№4215011, 4439350, 4443559, 5057468, 5189001, 5262012, 5266546, 5348710, 5431890 and 5730843, which are all entered in the description as the link. One of the preferred catalytic systems is that described in U.S. patent No. 5730843.

The system described in U.S. patent No. 5730843, has a rigid frame made of two essentially vertical coupled gratings, separated from each other and held fixed by means of many essentially rigid horizontal diaphragms and many essentially horizontal wire mesh tubes, mounted on grids, to form the set of passages for fluid between the tubes. When used as validator, at least part of the wire mesh tube is provided with a catalytic material. The catalyst in the tubes creates a reaction zone, which can be a catalytic reaction, and wire mesh creates a surface mass transfer to ensure fractional distillation. Spatial elements are used to change the density of the catalyst and the integrity of the system and boot.

One of the typical embodiments of the present invention shown in Fig.1. It includes depropanizer 10, in which, through the pressure line 101 is served With3+ stream containing propane, propylene, MAPD, more high-boiling olefins, and more high-boiling paraffins. The lower ndogoni of depropanizer contain4and more high-boiling materials, which are selected through line 102 for further processing. The head stream of depropanizer contains propylene, MAPD and propane, which are selected via the pressure line 103, condensed in the condenser 24, collect in the receiver 22 and is fed through a pressure line 106 in the first headspace single-pass reactor 20 containing a fixed bed of hydrogenation catalyst. Non-condensable components are removed through line 109. Typical working condition the flow returns to depropanizer as phlegmy through line 110. The hydrogen added to the reactor through a pressure line 104. In the reactor 20 part MAPD converted into propylene and propane. The first reactor can act as a protective layer to remove catalytic poisons, such as azine, mercury or methanol. The stream exiting the first reactor 20, selected through the pressure line 105 in the second single-pass reactor 30 containing a fixed bed of the same or similar catalyst for the hydrogenation, the reactor 20, and in which the additional amount MAPD turns into propylene and propane. The stream exiting the second reactor 30, is fed through a pressure line 106 in the distillation column reactor 40. If necessary add hydrogen through the pressure line 107. This variant of the invention may also be designed to use two main reactor 20 and 30 alternative by switching the downstream flow of depropanizer 10 between the reactors due to selection through the valve a and regulate the pressure line 105 through the valve 105A. In one such embodiment, the reactor serves as a protective layer for the column catalytic distillation until regenerate or change another catalyst reactor.

In a variant of this embodiment, is 20 and 30 may be made through the pipe 109. Operating temperatures are in the range of 100-250F. on the Contrary, in another embodiment of the invention the system can operate at higher pressures in all liquid models by pumping materials in line feed 106 to about 400 pounds per square inch and heated before entering the reactor 20 and 30. The temperature is in the same interval.

Distillation column reactor 40, as shown, contains a layer 41 of the same or similar catalyst that two reactors 20 and 30, but in this form, to act as a catalyst, and as a system for distillation. The distillation section 42 containing standard equipment for distillation, such as bubble cap plates, sieve trays or packing, is below the layer 41, to ensure the removal of all3-hydrocarbons in the main thread. The rectifying section 44 also contains standard equipment for distillation, such as bubble cap plates, sieve trays or packing, is above the layer 41 to ensure complete separation. Green oil containing not turned MAPD remove in the lower Neogene through the pressure line 108 and return in depropanizer, in which anyone With a3-material is taken as g is aporno line 111 and passed through a partial condenser at the top of the column 50, where C3-hydrocarbons condense and collect in receiver/separator 60. Not condensed material, including unreacted hydrogen, taken through the pressure line 112, and optionally hydrogen recycle. With3-the liquid out through the pressure line 113, and a portion returned to the distillation column reactor 40 in the form of phlegmy through the pressure line 114.

When using the process sequence of the present invention, the total selectivity to propylene at the starting cycle is 75%. In the final cycle, the selectivity is approximately 50%. This can be compared with about 50% of the starting cycle and 0% of the final cycle in the case of conventional vapor-phase converters.

In another embodiment of the invention, which is shown in Fig.2, the reactors 20 and 30 are removed. Raw materials With3fed directly to the distillation column reactor via a pressure line 106. Other parameters depropanizer and distillation column correspond to depropanizer and distillation columns Fig.1.

In another embodiment of the invention (shown in Fig.3) after distillation column reactor 40 is installed With3the divider 70. Head flow 111 enters directly into degu line 114. For other options work depropanizer 10 and distillation column 40 is similar to the variant in Fig.2. The head stream of the divider in the pressure line 112 contains a lighter material. Any condensed material condense in the condenser 80 and is collected in the collector/separator 90 for irrigation of the divider through the pressure line 124. Not condensed materials discharged through the pressure line 122. Propylene is withdrawn from the column below the downstream flow through the pressure line 123, and the propane is removed as the bottom of nedogona through the pressure line 128.

The above embodiments of the invention presented as a typical, but not limiting, examples of the flexibility provided by the method and circuit of the invention. For more options, configurations and conditions on the basis of the invention will be apparent to the skilled in this field specialist.

Claims

1. Method of removing methylacetylene and PROPADIENE from C3and more high-boiling hydrocarbon stream, comprising the stages of (a) the filing of a3and more high-boiling stream containing methylacetylene and PROPADIENE, in the first distillation column, where C3selected as the first head flow, and With thethe current and hydrogen in a distillation column reactor; (C) simultaneously in the specified distillation column reactor (i) contacting said methylacetylene and PROPADIENE with hydrogen in a reaction zone with a hydrogenation catalyst, resulting in these methylacetylene and PROPADIENE react with the specified hydrogen with the formation of propylene; and (ii) the Department contained propylene fractional distillation; and (d) discharge of the separated propylene together with any quantity of propane and lighter compounds, including unreacted hydrogen from the specified distillation column reactor as a second head of the stream.

2. The method according to p. 1, where the specified hydrogenation catalyst capable of acting as a system for distillation.

3. The method according to p. 2, where a stream containing unreacted methylacetylene and PROPADIENE, remove from the specified distillation column reactor as a second lower nedogona.

4. The method according to p. 3, where the specified second lower nedohin return specified in the first distillation column.

5. The method according to p. 1, including the additional stage (s) filing the specified second head stream in a third distillation column, in which propylene is separated from propane and any components boiling lower than propylene; and (f) selecting a side fraction from ukazom said first head flow serves, at least one single pass reactor with a fixed bed containing the catalyst hydrogenation, and he is in contact with the hydrogen to feed in the specified distillation column reactor reacted part of the specified methylacetylene and PROPADIENE with the formation of propylene.

7. Method of removing methylacetylene and PROPADIENE of enriched propylene stream comprising (a) feeding (1) a first stream containing propylene, methylacetylene and PROPADIENE, and (2) a second stream containing hydrogen, at least one single pass reactor with a porous layer containing a first hydrogenation catalyst, where part of methylacetylene and PROPADIENE reacts with hydrogen with the formation of propylene; (b) the flow goes from step (a) flow in a distillation column reactor in the area of raw materials; (C) simultaneously in the specified distillation column reactor (i) contacting the unreacted methylacetylene and PROPADIENE with hydrogen in a reaction zone with a second catalyst for hydrogenation, resulting react these olefins and acetylenic compounds with the specified hydrogen with the formation of propylene; and (ii) separating propylene fractional distillation; and (d) removing the separated propylene together with any Koli is NY-reactor in the form of the head of the stream.

8. The method according to p. 1, where the specified hydrogenation catalyst capable of acting as a system for distillation.

9. The method according to p. 1, where the specified hydrogenation catalyst contains from 0.05 to 5.0 wt.% oxide of palladium in the catalyst is aluminum oxide.

10. The method according to p. 8, in which hydrogen contained in the said second stream in an amount to provide a molar ratio of hydrogen to the specified methylacetylene and PROPADIENE from 1.05 to 2.5.

11. The method according to p. 8, in which the pressure in the upper part of this distillation column reactor is in the range between 90 and 315 pounds/square inch.

12. The method according to p. 8, in which the reaction is specified in a single-pass reactor with a porous layer takes place in the vapor phase.

13. The method according to p. 8, in which the flow coming from the stage (a), served in the second single-pass reactor with a porous layer in which the additional part of methylacetylene and PROPADIENE reacts with hydrogen to obtain propylene, and the flow coming out of the specified single-pass reactor with fixed bed, served on a stage (b).

14. The method according to p. 13, wherein said single-pass reactor with a porous layer acts as a protective layer to remove poisons these hydrogenation catalysts.

 

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