Method for obtaining hydrocarbons from synthesis gas

FIELD: oil and gas industry.

SUBSTANCE: invention relates to a method for obtaining hydrocarbon products, which involves the following stages: (a) provision of synthesis gas containing hydrogen, carbon monoxide and carbon dioxide; (b) reaction of conversion of synthesis gas to an oxygenate mixture containing methanol and dimethyl ester, in presence of one or more catalysts, which simultaneously catalyse the reaction of conversion of hydrogen and carbon monoxide to oxygenates, at pressure of at least 4 MPa; (c) extraction from stage (b) of an oxygenate mixture containing quantities of methanol, dimethyl ester, carbon dioxide and water together with non-reacted synthesis gas, introduction of the whole amount of the oxygenate mixture without any additional treatment to a stage of catalytic conversion of oxygenates (d); (d) reaction of oxygenate mixture in presence of a catalyst, which is active in conversion of oxygenates to higher hydrocarbons; (e) extraction of the outlet flow from stage (d) and separation of the outlet flow into tail gas containing carbon dioxide occurring from synthesis gas and carbon dioxide formed at stage (b), liquid hydrocarbon phase containing the higher hydrocarbons obtained at stage (d) and liquid water phase where the pressure used at stages (c)-(e) is mainly the same as that used at stage (b); besides, some part of tail gas obtained at stage (e) is recirculated to stage (d), and the rest part of tail gas is discharged.

EFFECT: this method is a method in which there is no recirculation of non-reacted synthesis gas to a synthesis stage of oxygenates and without any cooling of a conversion reaction of dimethyl ester to higher hydrocarbons.

6 cl, 2 ex, 1 tbl, 2 dwg

 

The present invention relates to a method for producing hydrocarbons, particularly gasoline.

In particular, the present invention relates to a combination process steps to produce compounds of gasoline from synthesis gas, where carbon dioxide is present in the synthesis gas formed during the above process, is separated from the liquid end connections of gasoline.

As we know, the gasoline synthesis proceeds in two stages: conversion of synthesis gas to oxygenates and the conversion of oxygenates in the gasoline product. These technological stage or can be combined, giving oxygenate intermediate product, such as methanol or mixtures of methanol to dimethyl ether (DME), and this oxygenate together with unreacted synthesis gas is fully enter into the next stage for conversion into gasoline, or the process may be carried out in two separate stages with intermediate separation of oxygenates, such as methanol, or crude methanol.

Useful oxygenates include methanol, dimethyl ether and higher alcohols and their ethers, but also can be used oxygenates such as ketones, aldehydes and other oxygenates.

In any case, the conversion of synthesis gas to oxygenates is accompanied by heat, because the conversion of synthesis gas to an oxygenate, and further conversion of the oxygenate is in the gasoline product are exothermic processes. Gasoline production scheme of the combined process is also discussed in U.S. patent No. 4481305. Hydrocarbons, particularly gasoline, produced by the catalytic conversion in two serially connected reactors synthesis gas containing hydrogen and oxides of carbon and having a molar ratio of CO/H2greater than 1 and at the beginning of the transformation of the molar ratio of CO/CO2from 5 to 20. In the first stage synthesis gas with high efficiency becomes oxygenate intermediate product containing predominantly dimethyl ether (DME), and in the second stage, the mixture turns into a gas by the total reaction scheme:

3H+3CO->CH3OCH3+CO2+Teplabout(1)

With aH3OCH3->2/n(CH2)n+H2O+Teplabout(2)

(CH2)nperformance, which provides a wide range of hydrocarbons, obtained at the stage of synthesis of gasoline. After separation of the hydrocarbon product of unreacted synthesis gas containing hydrogen and oxides of carbon is recycled to the stage of synthesis of oxygenates after CO2removed, at least partially, for example, by leaching from CO2.

The main objective of the invention to provide an improved circuit of the combined process for the production of valuable hydrocarbons boiling in the gasoline range fraction, rich in carbon monoxide synthesis gas, the process includes the synthesis of intermediate oxygenates and gasoline synthesis, without recirculation of unreacted synthesis gas phase synthesis of oxygenates and without removal of carbon dioxide from the intermediate oxygenate product synthesis before getting on the stage of synthesis of oxygenates and gasoline.

The present invention is based on the discovery, namely, that when carrying out the synthesis of oxygenates at high pressure, the conversion of synthesis gas to an oxygenate is almost complete, and based on further observation, namely, that a higher amount of carbon dioxide does not adversely affect the reaction in the conversion of oxygenates to higher hydrocarbons.

In its broadest embodiment, the present invention provides a method of gaining the hydrocarbon products, includes the following stages:

(a) providing a synthesis gas containing hydrogen, carbon monoxide and carbon dioxide;

(b) reaction of the conversion of the synthesis gas in the oxygenate mixture containing methanol and dimethyl ether in the presence of one or more catalysts which together catalyze the reaction of hydrogen and carbon monoxide to oxygenates, at a pressure of at least 4 MPa;

(c) removing from stage (b) oxygenate mixtures containing amounts of methanol, dimethyl ether, carbon dioxide and water together with unreacted synthesis gas, and the introduction of the total number oxygenate mixture without additional processing stage catalytic conversion of oxygenates (d);

(d) the oxygenate reaction mixture in the presence of a catalyst which is active in the conversion of oxygenates to higher hydrocarbons;

(e) separation of the effluent stream from step (d) in the tail gas, liquid hydrocarbon phase and a liquid aqueous phase,

where the pressure applied at stages (C)-(e), is essentially the same that is used in stage (b).

Synthesis gas, which can be used according to the present invention preferably provides to the ratio of N2/WITH about 1 and is introduced into the reaction in the presence of the catalyst for the formation of oxygenates, including the well-known catalysts on the education of methanol, for example, the catalysts containing copper oxide, zinc and aluminum, in combination with a dehydrogenation catalyst containing a solid acid, such as zeolite, alumina or silica - alumina.

In such a CO-enriched conditions, the reaction of water gas shift causes a strong increase of the conversion due to favorable thermodynamics, because the water generated at the stage of obtaining oxygenates, almost completely consumed by the reaction with CO, which produces hydrogen and carbon dioxide. The total reaction essentially becomes the reaction of hydrogen and carbon monoxide with the formation of DME+CO2. In such conditions can be achieved high levels of conversion, even when the synthesis gas contains appreciable quantities of CO2. In Fig.1 presents the equilibrium levels of conversion of synthesis gas, which are defined as

((H2+) Output/(H2+) Input)100%,

in the presence of a catalyst for the synthesis of oxygenates, which is active in the synthesis of methanol and dimethyl ether, and the reaction of water gas shift. It Is Evident From Fig.1 shows that theoretical rate of conversion of more than 90% is achievable at 7 MPa. At 13 MPa can be achieved conversion of more than 90%. At 7 MPa can be achieved conversion above 80% and even in the synthesis under pressure 4 MPa can be achieved conversion of 75%.

Therefore, when carrying out the research Institute synthesis of oxygenates at a pressure above 4 MPa according to the present invention can avoid the recycle synthesis gas, that provides an advantage.

The preferred pressure range for the application at the stage of synthesis of oxygenates is from 4 to 13 MPa.

The entire output stream extracted from the stage of synthesis of oxygenates containing mainly dimethyl ether and carbon dioxide with small amounts of methanol, hydrogen and carbon monoxide, is introduced into the next stage of the synthesis of gasoline.

Synthesis of gasoline carried out essentially at the same pressure, which is applied at the previous stage of the synthesis of oxygenates, in the presence of a catalyst which is active for the reaction conversion of oxygenates to higher hydrocarbons, preferably in C5+the hydrocarbons. The preferred catalyst for this reaction is known zeolite H-ZSM-5.

It is known that the reaction of the conversion of dimethyl ether and higher hydrocarbons is highly exothermic and requires either indirect cooling (for example, a boiling water reactor or fluidized bed) or dilution of the incoming reaction gas (for example, adiabatic reactor with fixed bed) with an inert gas or a reaction product, in order to control the reaction temperature.

In one embodiment of the present invention the exit stream from the stage of synthesis of oxygenates is diluted with an inert gas containing chiefly the m way carbon dioxide, which is recycled to the stage of synthesis of gasoline from the next next stage of separation of the products.

Carbon dioxide contained in the recycled gas, arises from unreacted synthesis gas and is formed as a side product during the synthesis of dimethyl ether and gasoline.

An additional advantage of the present invention is that carbon dioxide having a high heat capacity (Cp=48 j/K/mol), plays the role of solar heaters, which is favourable for the exothermic production of gasoline and reduces the level of recycling in comparison with known processes for the conversion of oxygenates in gasoline.

The exit stream from the reactor for the synthesis of gasoline contains hydrocarbons ranging from C1 to C11, water and carbon dioxide, and residual amounts of unreacted N2WITH and inert gases.

By cooling and condensation of the first liquid phase water to get the second liquid hydrocarbon phase mixture of gasoline and light petroleum gas (LPG), which is called the raw gas, and separate it from the gas phase containing carbon dioxide emerging from the synthesis gas and formed at previous stages, as described above. Raw gas can be subjected to further processing by traditional methods of obtaining low-boiling fractions of gasoline and a fraction of Legkov the petroleum gas (LPG).

As already indicated above in the present description, the portion of the gas phase containing carbon dioxide can be recycled to the stage of synthesis gas for temperature control.

The amount of recirculated gas are selected so that the concentration of oxygenates (Meon+DME) at the entrance to the reactor for the synthesis of gasoline was between 2 and 10 vol.%.

The method according to the present invention requires no separate preliminary or intermediate removal of carbon dioxide, thereby providing the advantage.

Another advantage of the present invention is that CO2present in the incoming stream of synthesis gas, and CO2formed at the stage of synthesis, can be removed after synthesis of gasoline essentially at the same pressure, which is applied at the stage of synthesis of oxygenates. This thread, in addition to increased CO2contains inert gases, such as N2and Ar, as well as combustible compounds in significant quantities: unreacted N2and, as well as nscontainerframe, mostly light, hydrocarbons, and therefore has a significant energy value.

As a result, part of the CO2-enriched gas phase, which is not refundable in the synthesis of gasoline can be burned, thereby providing a source of power that provides the provides the additional advantage of. An oxidizer for combustion may be air, preferably oxygen-enriched air, or, more preferably, the oxygen itself. The use of pure or nearly pure oxygen as the oxidant will give the resulting stream of essentially pure CO2containing small amounts of non-combustible inert gases such as nitrogen and argon. The pressure of the resulting stream of essentially pure CO2will be essentially the same as the pressure at the stage of synthesis of oxygenates.

Sequestration of carbon dioxide injected under high pressure into underground geological formations is designed to reduce the accumulation of greenhouse gases in the atmosphere. This sequestration is implemented in practice in many places, for example, in Beulah (North Dakota), where is the world's first enterprise with the use of coal, in which carbon dioxide is captured and stored using sequestration. Another example is the gas field Sleipner in the North sea, where carbon dioxide is recovered from natural gas with amine solvents and injected into deep mineralizovannyh aquifer.

Extraction of CO2at high pressure according to the present invention represents a significant advantage as it makes the sequestration CO2more economical, CPA is in the usual ways, such as methods of absorption of CO2liquid, such as, for example, Rectisol, Selexol or amine solutions, such as methyldiethanolamine. Besides the fact that these extraction processes are costly in terms of capital and operating costs, they usually reject CO2at pressures close to atmospheric, which causes the need for multiple stages of compression to achieve sufficient pressure 130 bar, or close to it, necessary for the implementation of sequestration.

Thus, the present invention makes purified CO2available at high pressure without the application of the aforementioned technologies for preliminary removal of CO2and only burning waste from the stage of gasoline synthesis gas.

The above described features and aspects of the present invention will be described in more detail in the following examples 1 and 2, involving drawing and Fig.2, which depicts the flow scheme specific options for performing the present invention.

Example 1

In a tubular reactor with an inner diameter of 19 mm was placed physical mixture of 49 g of a commercial catalyst for methanol synthesis, available at Haldor Topsee A/S under the trade name MC-131, and 21 g of a commercial catalyst for the synthesis of dimethyl ether, available at Haldor Topsee A/S under the trade name is receiving DMK-10. The catalyst was restored within 2 hours at 190C and 1.0 MPa flow (10 norms, liter/hour) 2% N2in N2. Then the reactor was fed a synthesis gas having the composition 1 in table 1 (Ar, listed in Table 1 as N2/Ar was used as an internal standard), at a rate of 100 rules. liter/hour, after which the pressure was increased to 8.8 MPa. When I installed the stable operating parameters, the composition of the effluent from the reactor stream is analyzed in real time by gas chromatography (composition 2 in Table 1).

Example 2

Referring to the below Fig.2 and Table 1, the synthesis gas having the composition 1 in Table 1, was applied to the reactor for the synthesis of oxygenates, which was boiling water under pressure of 8.8 MPa, getting the reaction mixture 2 enriched DME and CO2when the exit temperature of 260C. the Stream exiting the reactor for the synthesis of oxygenates, mixed with recycle stream 5', forming the stream 3, and was passed through the reactor for the synthesis of gasoline at 350C. Leaving the synthesis reactor of gasoline at a temperature of approximately 400C, stream 4 was cooled to 5C., separating the output stream in the gas phase 5, enriched in CO2, liquid phase 6 raw gasoline, and liquid water phase 7. Part of the gas phase 5 (5') is recycled into the reactor for the synthesis of gasoline to reduce the concentration of oxygenates in the stream that is included in the reactor SinTe is and gasoline, that serves as a means of reducing ekzotermicheskie reactor for the synthesis of gasoline. The rest of the gas phase 5 (5") is burned in oxygen 8 in the combustion chamber to produce heat and electricity, receiving the waste stream 9, more than 99% consisting of CO2when the pressure of 8.3 MPa.

Table 1
The number of the flow in Fig.2123456910
(mol.%)
H245.717.525.625.426.5
H2O21.40.1 2.737.4
CO43.19.414.114.014.6
CO27.541.950.249.751.22.162.399.6
N2/Ar0.140.280.40.40.40.20.4
Meon2.50.3
DME24.12.4the
C1-C21.53.05.15.25.3
C3-C4-1.31.31.69.4
C5+0.41.40.588.5
standards. m3/h102550950685120490528571357
kg/h 114

This example demonstrates that the synthesis gas containing significant amounts of CO2can be turned into fuel hydrocarbons, such as gasoline and LPG, with high efficiency and without the removal of the CO2. At the same time, this example illustrates that almost all of the CO2originally present in the synthesis gas, as well as CO2formed during the synthesis of oxygenates, can be extracted at high pressure close to the pressure applied during the synthesis, except for parasitic losses due to the pressure drop, etc. Extracted at a high pressure of CO2suitable for sequestration in contrast to the known processes capture CO2that CO2released at a much lower pressure, usually close to atmospheric, and requires several stages of compression, so it can be sequestrati.

1. The method of obtaining hydrocarbon products, comprising the steps:
(a) providing a synthesis gas containing hydrogen, carbon monoxide and carbon dioxide;
(b) reaction of the conversion of the synthesis gas in the oxygenate mixture containing methanol and dimethyl ether in the presence of one or more catalysts which together catalyze the reaction of transformation of toroda and carbon monoxide to oxygenates, at a pressure of at least 4 MPa;
(c) removing from stage (b) oxygenate mixtures containing amounts of methanol, dimethyl ether, carbon dioxide and water together with unreacted synthesis gas, and the introduction of the total number oxygenate mixture without additional processing stage catalytic conversion of oxygenates (d);
(d) the oxygenate reaction mixture in the presence of a catalyst which is active in the conversion of oxygenates to higher hydrocarbons;
(e) removing an effluent stream from step (d) and separation of the exit stream in the tail gas, containing carbon dioxide, resulting from the synthesis gas, and docsid carbon formed in stage (b), a liquid hydrocarbon phase containing obtained in stage (d) of the higher hydrocarbons, and a liquid aqueous phase, where the pressure applied at stages (c)-(e), is essentially the same as used in stage (b),
and part of the tail gas obtained in stage (e), recycled to the step (d), and the rest of the tail gas to dissipate.

2. The method according to p. 1, in which part of the tail gas remaining after stage (e), burn to get the gaseous product of combustion containing CO2.

3. The method according to p. 2, in which part of the tail gas remaining after stage (e), is burned with oxygen to produce energy and provide photocase 2at high pressure.

4. The method according to p. 2, in which the CO2subsequently sequestered.

5. The method according to p. 1, in which the pressure in stage (b) is between 4 and 13 MPa.

6. The method according to p. 1, in which the liquid hydrocarbon phase contains raw gasoline.



 

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10 cl, 1 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing ethylidene norbornene (ENB). The method comprises the following steps: a) feeding dicyclopentadiene into a first reactor for the thermal cracking of dicyclopentadiene to cyclopentadiene, carried out in inert heat transfer fluid having a boiling point >230 C, said thermal cracking being carried out at a temperature lower than the boiling point of said heat transfer fluid and lies between 200C and 300 C; b) feeding said cyclopentadiene produced at step a) into a second reactor in which said cyclopentadiene reacts with 1,3-butadiene to form vinyl norbornene (VNB); c) feeding said VNB produced at step b) into a third reactor in which a catalytic isomerisation of VNB to ethylidene norbornene (ENB) is carried out; d) collecting said ENB. Said step a) is characterised by that: i) said dicyclopentadiene fed to said step a) contains primary dicyclopentadiene from cracking containing up to 10 wt % of tetrahydroindene (THI), and recycled dicyclopentadiene containing tetrahydroindene (THI) recycled from said step b) of formation of vinyl norbornene; ii) said dicyclopentadiene containing said THI is fed into said heat transfer fluid and is in contact with it for a time of less than 1 minute; iii) the formed cyclopentadiene vaporises into the gas phase established above said liquid phase and is continuously removed from said first reactor; iv) a part of said heat transfer fluid substantially free of dicyclopentadiene and rich in THI is continuously fed into a fractionation column, said THI being collected at the top of said column and said heat transfer fluid being collected at the bottom of said column; v) said heat transfer fluid purified in step iv) is recycled to said first reactor of said step a).

EFFECT: high efficiency of the method.

15 cl, 2 ex, 1 dwg

FIELD: oil and gas industry.

SUBSTANCE: invention refers to gas industry and can be used at gas condensate fields, immediately at sites of gas preparation for transportation or at centralised sites of preparation of instable gas condensate for transportation or processing. The invention refers to the method of obtaining liquid ethane from instable gas condensate, which involves separation of gas condensate in a rectifying column into three flows, two gas ones - methane and ethane, and one liquid - deethanised condensate, ethane gas flow separation with a side shoulder of the rectifying column, which is located on the level of gaseous phase containing ethane free from methane, and further condensation of ethane flow and extraction of liquid ethane from condensed ethane flow.

EFFECT: enlarging the range of products, improving their quality and low-temperature properties.

1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of separating an isopentane-pentane-hexane fraction during an isomerisation process, consisting of a first fractionation column for preparing material, from which the ballast product contained in the material is separated with the distillate. The residue from the bottom of the fractionation column is taken for conversion of pentanes and hexanes into isomers in an isomerisation reactor. Isomerisation products are fed into a second fractionation column for debutanisation, from where butane is removed from the top of the column and the isomerisation product is removed from the bottom of the column, said product containing reaction isomers obtained during the reaction, which are fed for separation into a third fractionation column for depentanisation, from which isopentane, recycled pentane and a hexane fraction are successively removed from the top. The recycled pentane is returned into the isomerisation reactor. The method is characterised by that the starting material used is a 75-85C fraction of straight-run gasoline, and the ballast product removed from the top of the first fractionation column is isopentane contained in the material; reaction isopentane is removed from the top of the third fractionation column for depentanisation as a distillate or with the first side cut. Excess butane is removed as the distillate. Pentane is removed with the second side cut of the depentanisation column and fed into the isomerisation reactor as a recycle stream. A mixture of isohexane and normal hexane is removed from the bottom of the depentanisation column and then fed as material into an additional fourth fractionation column for deisohexanisation, from which the isohexane fraction is removed with the distillate and recycled hexane is removed with the side cut and then fed for re-conversion into the isomerisation reactor, and higher-boiling components are removed with the residue.

EFFECT: use of the present method enables to cut the amount of energy spent in the isomerisation process on producing isoparaffins, widens the range of products and provides flexibility of the process and purity of the end products.

2 cl, 4 tbl, 1 dwg

FIELD: chemistry.

SUBSTANCE: method includes supply of said output flow into fast cooling column; supply of circulating water flow into fast cooling column and flowing of water flow in column in cascades downward; dispersion of second water flow to form spray from water drops, with said spray being supplied into channels for steam, through which flows output from reactor pass, with spray is dispersed directly above openings of plates, placed in fast cooling column; and contact of output from reactor flow with water flow and spray from water drops to remove catalyst particles from output flow, with formation of fast cooled output from reactor flow and flow of water and solid particles, discharged from column.

EFFECT: application of claimed invention makes it possible to increase efficiency of removal of fine-disperse particles of solid catalyst from product flow, output from reactor.

10 cl, 3 dwg

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