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INVENTION
Patent of the Russian Federation RU2278101
METHOD OF INTEGRATED PROCESSING OF NATURAL GAS WITH RECEIVING FRESH WATER AND FUEL AND INSTALLATION FOR ITS IMPLEMENTATION
The name of the inventor: Fedorov Evgeniy Alexandrovich (RU); Lishchiner Joseph Izrailevich (RU); Malova Olga Vasilievna (RU)
The name of the patent holder: Fedorov Evgeniy Alexandrovich (RU)
Address for correspondence: 105568, Moscow, ul. Chelyabinsk, 23, building 2, ap.253, E.A.Fedorov
Date of commencement of the patent: 2004.07.16
Use: petrochemistry. Essence: synthesis gas is obtained by gas-phase oxidative conversion of natural gas with air oxygen, catalytic conversion of synthesis gas to catalyst, after cooling and separation of which the liquid phase is sent to a gasoline production reactor, in order to reduce the cost of production in the synthesis reactor, catalytic methanol To the reactor for producing high-octane gasoline components that are stabilized and separated into liquid products and fatty gas sent to the oligomer-gasoline production reactor, the liquid products of the reactors for producing high-octane gasoline components and oligomer-gasoline are then combined, and the mixture is stabilized, Of all synthesis reactions, separated separately after separation, combined and fed to the fresh water preparation unit, and the resulting nitrogen is stored for partial storage in the processing cycle and during storage of the synthetic fuel, unreacted lean synthesis gas from the methanol production unit is used to supply methanol to the injectors Reactor for obtaining high-octane gasoline components, and unreacted gases from the oligomer-gasoline production reactor are sent to the synthesis gas generator. And a plant for implementing the process, consisting of blocks for synthesis gas synthesis, catalytic conversion of synthesis gas to catalyst, and production of gasoline, is claimed with two separate reactors for producing high-octane gasoline and oligomer-gasoline additives, the unit is further provided with a fresh water preparation unit and a nitrogen collection unit , Wherein the nozzles of the reactor for producing high-octane gasoline components are pneumohydraulically connected to an intermediate methanol collecting tank and methanol synthesis reactor of the methanol production unit, and the oligomer gasoline production reactor is pneumatically connected to the synthesis gas production unit. The technical result: the creation of a method for the joint production of fuel and fresh water.
DESCRIPTION OF THE INVENTION
The invention relates to methods for complex processing of natural gas and air with simultaneous production of drinking and agricultural water, high-octane gasoline components and gases.
A method for complex processing of sea water with the production of fresh water and valuable mineral components is known. The method includes successive stages of mechanical filtration, separation of elements and salts from those present in sea water and from brines and fresh water [1].
The main drawbacks of the method of RF patent No. 2089511 are the cumbersomeness of the equipment, low production efficiency at high energy costs, high production costs of fresh water.
The technology of processing natural gas into synthetic diesel and jet fuel is known at small-sized low-pressure plants [2].
The known technology includes two main successive steps: synthesis gas production by methane conversion and Fischer-Tropsch synthesis, which allows obtaining high yields in the single-pass process with the C 7 -C 20 fraction. If necessary, the standard fractionation stage can be included in the technology.
The main disadvantages of the technology are low productivity, a narrow range of products (including up to 30% of low-octane gasoline plus fractions that require additional processing), a high cost of the process as a whole with the disposal of water as a waste of the main production.
A method for obtaining motor fuels from a carbonaceous feedstock with a stepwise production of a final product from a synthesis gas feedstock is also known. The gas stream after the first-stage reactor is cooled and separated into a liquid fraction and a gas phase containing unconverted synthesis gas and dimethyl ether (DME) components, whereupon DME is separated from the liquid fraction and the gas phase is divided into 2 streams, one is blended With synthesis gas and fed to the same reactor of the first stage. The second gas stream is fed to a second stage where, upon contact with a catalyst consisting of a ZSM-5 zeolite and a metal oxide component, DME and synthesis gas components are converted to a gasoline fraction, gaseous hydrocarbons and an aqueous fraction (Ru 2143417) [3].
The main disadvantages of this method of obtaining motor fuels from carbon-containing raw materials under the RF patent No. 2143417 are: the need to use oxygen in the synthesis gas production, which in turn requires the creation of an oxygen farm with significant capital investments and high operating costs, low DME output, and therefore gasoline Fraction, high cost of the process, high degree of contamination of the water fraction and its subsequent utilization together with gaseous hydrocarbons.
A method for obtaining motor fuels is known in which synthesis gas is produced by a non-catalytic gas-phase oxidative conversion of natural gas by air oxygen at a temperature of 800-1500 ° C and a pressure of 1-10 MPa. Then, the synthesis gas is catalytically converted in a dimethyl ether synthesis reactor, followed by cooling the resulting gas mixture and separating it into a liquid and a gas phase. At the same time, dimethyl ether is separated from the liquid phase and sent to a catalytic gasoline synthesis reactor, and the gas phase containing unconverted synthesis gas components is sent to a re-catalytic conversion to an additional dimethyl ether synthesis reactor without mixing with the starting synthesis gas (Ru 2226524) [4] .
The method makes it possible to increase the yield of dimethyl ether and, correspondingly, of the gasoline fraction and to reduce the process costs through the use of atmospheric oxygen, but does not solve the problem of the complex nature of natural gas processing by utilizing waste that includes unconditionally valuable commodity product - water, and the overall total production cost remains high.
The technical task of the claimed group of inventions is to improve the quality of water, reduce the cost of production, improve the ecology of the environment, increase the efficiency of the process.
The technical task is achieved by the method of complex processing of natural gas, which involves the production of fresh water and fuel, including synthesis gas production by gas-phase oxidative conversion of natural gas by air oxygen, compression of synthesis gas, its further purification from residual oxygen and moisture, subsequent catalytic conversion of synthesis gas to Catalyzing, cooling and separating the catalyst, directing the liquid phase of the catalyst to the gasoline production reactor and separating the water in the separator receivers, characterized in that, in order to improve the quality of water, reduce the cost of production, improve the ecology of the environment and improve the efficiency of the process, the reactor Synthesis of the catalyst, the methanol formed is sent to reactors for the production of high-octane gasoline components where, in the presence of a zeolite catalyst at a pressure of 0.7-1.0 MPa and a predetermined temperature, high-octane gasoline components are obtained that are separated into liquid condensate and fatty gas sent to the oligomer- Gasoline, and the liquid condensate is divided into an aqueous layer and liquid organic products combined with the previously obtained oligomer gasoline and supplied to the gasoline stabilization unit, and the water formed during all stages of product synthesis is separately withdrawn, combined and fed to the block after separation Fresh water preparation where methanol and fatty hydrocarbon residues are distilled from it, subjected to bio-purification and mineralization, and the nitrogen produced during the process is stored and partially used in the production cycle, while unreacted gases from the oligomer gasoline production reactor are sent to a synthesis- Gas, and depleted synthesis gas from the reactors for producing high-octane gasoline components is fed to the methanol atomization in the nozzles of these reactors.
The set technical task is achieved by installing a natural gas generator for complex processing to produce fresh water and fuel containing a synthesis gas production unit including air and natural gas purification and compression units, a synthesis gas generator, a synthesis gas compression unit, a methanol production unit Including reactors for post-treatment of synthesis gas, methanol synthesis reactors filled with catalyst and series-mounted heat exchanger, an intermediate tank for collecting methanol, a block for obtaining high-octane gasoline components, including reactors filled with zeolite catalyst, the nozzles of which are pneumohydraulically connected to an intermediate methanol collecting tank and synthesis reactors Methanol, a refrigerator, a three-phase separator, an oligomer gasoline production unit comprising an oligomer gasoline production reactor pneumatically connected to a synthesis gas block, a gasoline stabilization unit including a stabilization column, a commercial gasoline collection tank, a fresh water preparation unit including a distillation unit Residual methanol and hydrocarbons, units for bio-purification and mineralization of water, tanks for collecting water, nitrogen collection.
The basis for the method of complex processing of natural gas with the production of fresh water and fuel is the development of highly efficient technologies for the production of synthesis gas, methanol and high-octane gasoline components (VOC), which enable to solve the problem of obtaining an additional source of drinking and agricultural water with environmental protection in an environmentally friendly manner. The method is original, surpasses the world analogues at the cost, depth and complexity of processing raw materials with a high degree of use of end products and energy-tightness of the whole process.
A basic block diagram of a complex natural gas processing unit including the production of fresh (drinking) water is presented in FIG. 1
FIGS. 2 to 7 are diagrams of individual units of a complex natural gas processing unit.
The complex natural gas processing unit comprises a synthesis gas generation unit (1) (BS-G), a methanol production unit (7), a high-octane gasoline component producing unit (25), an oligomer gasoline production unit From the fatty gases formed after the BBBB unit (BB-B), the gasoline stabilization unit (BSB), the fresh water preparation unit (42), the nitrogen collection container (48) formed during the process.
The gas synthesis synthesis unit (1) includes the air cleaning and compression unit (2), the purification, conditioning and compression of natural gas unit (3), the air and natural gas mixing unit (4), the synthesis- Gas, a synthesis gas compression unit (6) (see Fig. 2).
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The block (7) for producing methanol BM (see Figures 1 and 3) includes the synthesis gas (SG) after-treatment reactors (8) and (9) from residual oxygen and moisture, refrigerators (10-12), separator receivers (13 -15), methanol synthesis reactors (16-18), mounted in series, a heat exchanger (19) for heating the gas feedstock, an intermediate tank (20) for collecting methanol.
The high-octane gasoline component production unit (25) (see Figures 1 and 4) includes a methanol feed pump (21), a recuperative heat exchanger (22), reactors (23-24) for producing high-octane gasoline components (VKB), a water cooler (26), a three-phase separator (27), a regeneration gas heating furnace (28), a regeneration gas compressor (29).
The unit (30) for producing oligomer gasoline from fatty gases (BO-B) includes a liquid gas compressor (31), a refrigerator (32), a separator (33), a regeneration gas heating furnace (34), a petrol oligomerization reactor (35) A compressor (36) for supplying regeneration gas (FIGS. 1 and 5).
The gasoline stabilization unit (37) (FIGS. 1 and 6) includes a stabilization column (38), an air cooler (39), a reflux tank (40), a tank (41) for collecting commercial gasoline.
The fresh water preparation unit (42) includes a methanol distillation unit (43) for removing methanol and fatty hydrocarbon residues, a bio-cleaning unit (44), a mineralization unit (45), and an improvement in the taste of water, an intermediate tank (46) for collecting water , A storage tank (47) for water. (Figures 1 and 7).
Below is a description of the operation of the plant and the method for complex processing of natural gas. After passing through the purification, conditioning and compression unit (3), the natural gas is mixed in a mixing unit (4) with air passing through the air cleaning and compression unit (2) of the synthesis gas generating unit (1) in a ratio of 1: 5 or 1: 6, and then goes to the synthesis gas generator (5), where synthesis gas is formed at a temperature of 850-900 ° C (or 2000 ° C) (the ratio of H 2 : CO = 2,1: 1 or 1,8: 1, respectively). Then, the resulting synthesis gas at 260 ° C, a pressure of 4.5-5.0 MPa and a space velocity of 5000 h -1 -4000 h -1 comes from the synthesis gas compression unit (6) of the synthesis gas production unit (1) at Pressure of 5.0 MPa to the reactor (8) after purification of the synthesis gas from the residual oxygen (up to 0.5%) if the oxygen concentration in the synthesis gas exceeds 0.5% vol. The reactor (8) for post-treatment of synthesis gas from the residual oxygen is shell-and-tube, loaded with an aluminomickel-copper (or alumopalladium) catalyst. The loading volume is 3.0 m 3 (3.6 t) at a gas feed rate of 8000 h -1 . The operating temperature is 200-240 ° C. After the reactors (8-9), (16-18), water coolers (10-12) and separator receivers (13-15) are provided to trap the water formed during the cleaning.
Thus, synthesis gas purged of residual oxygen enters the intermediate reactor (9) for its further purification from the residual moisture (it is also necessary for post-cleaning with soot, if available). The reactor (9) is a vertical cylindrical apparatus loaded with adsorbent-silica gel. The amount of loading is determined by the performance of the installation. The operating temperature of the reactor is 40-50 ° C. Two parallel switched reactors are in operation, one of which operates, and the other is in the regeneration stage of the adsorbent as its adsorption capacity is lost. Regeneration is carried out in a nitrogen flow of 200-300 h -1 at a temperature of 140-160 ° C.
Further, the synthesis gas is sent to the first of the three reactors (16-18) for the synthesis of methanol BM, incidentally heated to 160-180 ° C in the heater built into the reactor.
The reactor is shell-and-tube, loaded with an aluminum-zinc-copper catalyst. Operating temperature is 240-250 ° C.
The catalyst for the synthesis of methanol is activated once for the entire lifetime, so the hydrogen economy is only needed for the period of preparation of the installation for operation. Reactors (16-18), mounted on a "cascade" scheme, without preheating the synthesis gas. After each reactor, water coolers (10-12) and separator receivers (13-15) are provided to collect the methanol formed.
The process of obtaining methanol is accompanied by the release of thermal energy (110.8 kJ per mole using pure methanol or 3090000 kJ per ton of methanol-crude), which can cause an excessive temperature rise, which leads to an irreversible decrease in the activity of the catalyst. The maximum permissible temperature is 270 C. For a partial removal of the reaction heat and for the system to be fed by synthesis gas, cold (60-80 ° C) synthesis gas is fed to the intertubular space of the reactors after purification and drying.
The methanol production unit (7) also comprises a heat exchanger (19) for heating the gas feed (syngas) and an intermediate tank (20) for collecting methanol. From the receiver-separators (13-15) of all reactors in the unit (7), methanol enters the intermediate tank (20) to collect methanol. Next, methanol from the intermediate tank (20) of the unit (7) is supplied by the methanol feed pump (21) after heating in the recuperative heat exchanger (22) to 180-220 ° C into the reactors (23-24) for producing high-octane gasoline components (BVKB) of the block (25 ) Of obtaining BVKB. The depleted synthesis gas is then fed to atomize methanol in the nozzles of the reactor for producing high-octane gasoline components (VKB). The reactors (23-24) for obtaining high-octane gasoline components of the VKB production unit (25) operate alternately with an inter-regeneration run of not less than 500 hours, are filled with a zeolite catalyst containing a pentasil type zeolite. Catalytic conversion is carried out at a pressure of 0.7-1.0 MPa. The total volume of catalyst in each reactor (23-24) for the production of WKB is at least 3.3 m 3 .
The temperature regime of the reactors (23-24) is regulated to maintain a certain conversion of raw materials throughout the conversion cycle. The heat removal of the exothermic reaction occurs through the internal surface of the reaction space. The heat flow is then used as a heat source in a plant for heating the recycle gas, supplying the heat exchangers and heating the cube of the stabilization column (38) of the gasoline stabilization unit (37).
Regeneration of the catalyst is carried out at a pressure of 0.7-1.0 MPa with a nitrogen-air mixture circulated by a compressor.
To heat the catalyst regeneration gases, heat exchangers and furnaces (not shown schematically in FIG. 1) serve to heat the regeneration gas. The regeneration time is 100-120 h, the service life of the zeolite catalyst is at least 2 years.
The reaction products (catalyst) with a temperature of 420-430 ° C from the reactors (23-24) pass the heat recovery heat exchanger (22), then after cooling in the water cooler (26) of the BVKB production unit (25), the catalyst is separated in a three-phase separator (27 ) Of the BVKB production unit (25). The fatty gases enter the oligomerization reactor (35) of the oligomer gasoline (BO-B) production unit (30) containing the liquid gas compressor (31), the refrigerator (32), the separator (33), the regeneration gas heating furnace (34) and Compressor (36) for supplying regeneration gas. The liquid condensate is stratified and settled in the separator (33), the aqueous layer is separated and the liquid organic products are directed to the preheating in the heat exchangers and to the column (38) for stabilizing the gasoline stabilization unit (37) operating at a pressure of 1.2-1.4 MPa. In the reactor (35) of the BPO-B block (30) at a pressure of 2 MPa, the conversion of the olifins takes place to form oligomer-gasoline. In the reactor (35), the same zeolite catalyst can be used. The unreacted gases from the top of the oligomer gasoline production reactor (35) of the BPO-B production unit (30) are sent to the synthesis gas generator (5) of the synthesis gas production unit (1), and the liquid organic products formed are combined with unstable gasoline from a three-phase Separator (27) of the BVCB production unit (25) and are sent to the stabilization column (36) of the gasoline stabilization unit (37). The operating temperature of the reactor (35) of the unit (30) of the BPO-B is 340-380 ° C, the volumetric flow rate of the liquefied gases is 2-4 h -1 .
The filtration element of the cleaning and air conditioning unit BS-G provides purification from oil and mechanical particles.
The generator (5) of the synthesis gas BS-G provides the following gas composition:
A generator (5) of synthesis gas operates at a pressure of up to 1 MPa, an operating temperature of not more than 1000 ° C (in the case of catalytic conversion of methane to synthesis gas). The synthesis gas temperature at the outlet from the heat exchanger is no more than 30-50 ° C.
Depending on the tasks and the required capacity, several generators can be connected in the BS-G, including with different types of reactors.
From the bottom of the column (38) stabilizing the gasoline stabilization unit (37), stable gasoline is selected and, after cooling, is removed from the unit as a commercial product in a container (41) for collection of marketable gasoline.
The overhead of the stabilization column (38) is cooled in the air cooler (39) of the gasoline stabilization unit (37) and collected in the reflux tank (40) of the gasoline stabilization unit (37). The liquid organic condensate is partially supplied by the pump (for conditionally not indicated) to the irrigation of the column (38) of the BSB unit (37), and a predetermined amount is circulated to the reactor (23-24) for producing the WKB of the BBBB production unit (25). The use of two parallel blocks (25) for the production of BVKB and (30) the production of BPO-B oligomer gasoline increases the yield of water.
The water is supplied to the distillation unit (43) of the methanol and fatty hydrocarbon residues of the HPV fresh water preparation unit (42) and then fed to the bio-cleaning unit (44), where cleaning is completed.
The unit (45) of mineralization and improving the taste qualities of the block water (42) HPV completes the process of obtaining drinking and agricultural water. The unit (42) contains intermediate and storage tanks (46-47) of water.
The installation is equipped with an automatic control system that provides trouble-free automatic shutdown in case of failure of the performance of individual elements.
Specific examples of the implementation of the claimed method, according to the above described process diagram and the operation of the plant, are given below, containing specific examples of the modes of implementation of the individual process steps, which, accordingly, do not limit it.
Example 1
The feedstock-natural gas is mixed with air in a ratio of 1: 5-6, after which the mixture enters the converter of gas-phase oxidative conversion of natural gas by air oxygen, where at 850-2000 ° C a synthesis gas with the ratio H 2 : CO = 1.8-2.1: 1. The resulting synthesis gas after the compression unit at a pressure of 5.0 MPa is fed to the reactor for its further purification from the residual oxygen if the oxygen concentration in the synthesis gas exceeds 0.4% by volume at a gas feed rate of 8000 h -1 and an operating temperature of 200 -240 ° C. After the purification reactor, the synthesis gas is cooled and fed to a receiver-separator to trap the water formed during the purification.
Then, the resulting synthesis gas at 260 ° C, a pressure of 4.5-5 MPa and a space velocity of 4000-5000 h -1 is directed to catalytic conversion to the methanol synthesis reactor. The resulting catalyst is cooled. Then it is divided into liquid (methanol-crude) and gas phase. The raw methanol enters the catalytic conversion reactor, where at 380-430 ° C, a pressure of 0.6-1.0 MPa is contacted with a catalyst containing a pentasil-type zeolite and a metal oxide component, as a result of which water and hydrocarbons (liquid and gaseous) are formed in the ratio 1: 0.5 for raw materials - natural gas. Gaseous hydrocarbons are sent to the oligomer gasoline production reactor. Water, formed at all stages of synthesis, is combined and fed to the fresh water preparation unit.
Example 2
The natural gas is mixed with air in a ratio of 1: 6 and fed to the converter, where at 2000 ° C synthesis gas is formed in the ratio H 2 : CO = 1.8: 1. Then, the resulting synthesis gas at 260 ° C, a pressure of 4.5 MPa and a space velocity of 4000 h -1 enters the methanol synthesis reactor. The resulting methanol enters the conversion reactor, where at 430 ° C, a pressure of 1.0 MPa is contacted with a catalyst containing a pentasil-type zeolite, resulting in water and hydrocarbons in a ratio of 1: 0.4 to natural gas.
A basic block diagram of a plant for producing fresh water by complex processing of natural gas is shown in FIG. 1.
The estimated capacity of the installation in the example above is up to 16 tons per year of water and up to 6.3 tons per year of WKB (or up to 10 tons per year of gasoline).
The natural gas cleaning unit BS-G provides a sulfur content of 0.1 ppm in the form of H 2 S, chlorine is absent
INFORMATION SOURCES
1. Patent of the Russian Federation No. 2089511, C 02 F 1/42, publ. 10.09.97. Bul number 25.
2. Kagan DN, Lapidus AL, Krylova A.Yu. Development of low-stage technology for processing natural gas into synthetic diesel and jet fuel at small-size low-pressure plants. - Gas chemistry in the XXI century. Problems and prospects (Works of the Moscow seminar on gas chemistry 2000-2002). M., 2003, p.131-170.
3. Patent of the Russian Federation No. 2143417, C 07 C 1/04, 41/06, publ. 1999. Bulletin №12.
4. Patent of the Russian Federation No. 2226524, C 07 C 1/04, 41/06, 43/04, C 10 G 3/00, publ. 10.04.2004. Bul No.10.
CLAIM
1. A method for complex processing of natural gas, which involves the production of fresh water and fuel, including synthesis gas production by gas-phase oxidative conversion of natural gas by air oxygen, compression of synthesis gas, its further purification from residual oxygen and moisture, subsequent catalytic conversion of synthesis gas to catalyst, Cooling and separating the catalyst with the direction of the liquid phase of the catalyst to the gasoline production reactor and separating the water in the separator receivers, the methanol formed from the catalytic synthesis reactor being sent to the reactors for producing high-octane gasoline components, where in the presence of a zeolite catalyst at a pressure of 0.7-1, 0 MPa and a given temperature, high-octane gasoline components are obtained which are separated into liquid condensate and fatty gas sent to the oligomer gasoline production reactor, and the liquid condensate is separated into an aqueous layer and liquid organic products combined with the previously obtained oligomer gasoline and fed to the block Stabilizing the gasolines, while the water formed during all stages of product synthesis is separately withdrawn, combined and fed to the fresh water preparation unit after separation, where methanol and fatty hydrocarbon residues are distilled from it, subjected to bio-purification and mineralization, and the nitrogen produced during the process Are supplied for storage and partial use in the technological cycle, whereby unreacted gases from the oligomer gasoline production reactor are sent to the synthesis gas generator, and the depleted synthesis gas from the reactors for producing high-octane gasoline components is fed to atomize methanol in the injectors of these reactors.
2. A plant for complex processing of natural gas in the manner of claim 1, obtaining fresh water and fuel, comprising: a synthesis gas production unit including air and natural gas purification and compression units, a synthesis gas generator, a synthesis gas compression unit, a production unit Methanol synthesis reactors, methanol synthesis reactors filled with catalyst and series-mounted heat exchangers, an intermediate tank for collecting methanol, a block for producing high-octane gasoline components including zeolitic-filled reactors, the injectors of which are pneumohydraulically connected to an intermediate methanol collecting tank and reactors Synthesis of methanol, a refrigerator, a three-phase separator, an oligomer gasoline production unit comprising an oligomer gasoline production reactor pneumatically connected to a synthesis gas block, a gasoline stabilization unit including a stabilization column, a commercial gasoline collection tank, a freshwater preparation unit comprising a unit Distillation of residual methanol and hydrocarbons, units for bio-purification and mineralization of water, tanks for collecting water, nitrogen collection.
print version
Date of publication 01.01.2007гг
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