Method of methanol obtaining

FIELD: chemistry.

SUBSTANCE: invention pertains to the method of methanol obtaining from a concentrated mixture of hydrogen and carbon oxides with the following components in vol %: H2 - 62.0-78.5; Ar - 0.02-0.07; N2 - 0.05-2.2; CH4 - 1.0-3.5; CO - 10.4-29.5; CO2 - 3.2-10.7. The methanol is obtained by concentrating it in a copper containing catalyst at high temperature and pressure in two stages. The gas mixture from the reformer is divided into two streams in volume ratios of 100 : (1-50), one of which is in direct contact with the catalyst in the flow reactor at the first stage, at temperature of 200-285°C, pressure of 5-15 MPa and volume rate of 800-2000 h-1. The other stream is mixed with a cycled gas in volume ratio of 10 : (10-100) and with volume rate of 2500-10000 h-1. This stream is then channelled to the second stage, with separation of methanol and water on each stage in corresponding devices.

EFFECT: increased production of methanol and increased efficiency of the process.

1 tbl, 1 dwg

 

The invention relates to the field of organic synthesis, in particular the production of methanol from hydrogen and carbon oxides.

Known [GB No. 1159095, IPC SS 32/00, Appl. 18.08.65,, publ. 23.07.69,] the method of producing methanol, comprising the reaction of carbon oxides with hydrogen under a pressure of 1.0-15.0 MPa (preferably from 4.0 to 8.0 MPa), the temperature of 160-300°With (preferably from 190 to 270°C), flow rate 7000-25000 h-1in the presence of a catalyst containing the oxides of copper and zinc and at least one trudnovosplamenjaemy the metal oxide of the second - fourth groups of the periodic system of elements DI Mendeleev, separation of methanol from the reaction mixture and recycling the unreacted in the synthesis of methanol substances. As a raw material using a mixture of hydrogen oxide and carbon dioxide, in which the content of CO2varies in the range of 1-20 vol.% (preferably 3-12%). In the reaction gas in contact with the catalyst, the volume ratio of hydrogen to the sum of the oxides of carbon 1.3 to 3.0 times the stoichiometric.

The disadvantages of this method include low specific capacity of the copper-zinc catalyst, and the high energy cost of recycling the gas mixture.

A known method of producing methanol [RU No. 2181117, IPC SS 29/154, 31/04] contacts g of the gas mixture, containing oxides of carbon and hydrogen, with a copper-containing catalyst at a temperature of 190-290°C, pressure of 5.0-10.0 MPa and flow rate 4500-100000 h-1and the source gas mixture containing 1.0 to 33,7% vol. oxide of carbon, 0.3 to 22,5% vol. carbon dioxide, when the volume ratio of hydrogen to the sum of the oxides of carbon, equal 1,91-the ceiling of 5.60, and 0.5 to 50 vol.% nitrogen, sequentially passed through a cascade of two reactors (tubular type in one stage, and methanol and water are separated after each reactor.

Consider the cascade method allows to significantly increase the performance of the catalyst, however, the implementation of the proposed technical solutions associated with a significant material cost and technically complex. In addition, it is possible a significant reduction in lifetime of the copper-zinc catalyst, and performance methanol installation depends on the amount of flow reactors.

The closest set of features of the claimed invention is a method of producing methanol [SU # 1442514, IPC SS 29/15, 31/04] contacting a mixture of hydrogen and carbon oxides with copper-containing catalyst at elevated temperature and pressure in two stages, followed by separation of methanol, with the aim of increasing the specific productivity of the catalyst and the forgiveness process flow diagrams, in the first stage, the gas mixture containing 0.7-30,0%vol., CO20,3-23,6% vol. when the ratio of CO:CO2equal (0,03-87):1, in contact with the catalyst in reactor consisting of one flow-through reactor or a cascade of two reactors, and in the second stage the process is conducted at a concentration of CO2in the incoming gas mixture of 0.4 to 20.0 vol.% and the ratio of CO:CO2equal to (0.25 to 55), followed by separation of the methanol and water known techniques in multiple devices or a single for both stages of the device.

The disadvantage of this method of producing methanol is the variability of specific performance of the catalyst by varying the content of carbon dioxide in the gas mixture.

An object of the invention is the improvement of the technological scheme of the process while maintaining its high level of efficiency.

This object is achieved in that in the proposed method, methanol is synthesized from convertible mixture of hydrogen and carbon oxides by contacting with a copper-containing catalyst at elevated temperature and pressure in two stages, with the aim of increasing the specific productivity of the catalyst gas mixture from the furnace reformer composition, vol.%: H2- 62,0-78,5; Ar - 0,02-0,07; N2- 0,05-2,2; CH4- 1,0-3,5; CO - 10,4-19,5; CO2- 3,2-10,7 Affairs is conducted on two threads in a volume ratio of 100:(1-50), one of the first stage directly in contact with the catalyst in a flow reactor at a temperature of 200-285°C, a pressure of 5-15 MPa and flow rate 800-2000 h-1and the other is mixed with the circulating gas in a volume ratio of 10:(10-100) and with a bulk velocity 2500-10000 h-1sent to the second stage with the release of methanol and water at each stage in the respective devices.

Distinctive features of the proposed two-stage method of producing methanol are as follows:

- converted gas composition, vol.%: H2- 62,0-74,5; Ar - 0,02-0,07; N2- 0,05-2,2; CH2- 1,0-3,5; CO - 10,4-29,5; CO2- 3,2-10,7 supplied with the furnace reformer, is divided into two streams in a volume ratio of 100:(1-50), one of which is in direct contact with the catalyst in a flow reactor, and the second is directed to mix with the gas circulation and then into the circulation reactor;

- volume ratio and converted circulating gas before mixing is equal to 10:(10-100).

It is well known that the processing of the synthesis gas containing carbon monoxide more than 30 vol.% and nitrogen over 40% vol. uneconomical. For this reason, the proposed method uses the synthesis gas, in which dosage WITH maintained below 25 vol.%, and the volume ratio of N2/(CO+CO2) is in the range from 2 to 5.

D. the I optimal concentration of CO 2can be used in its submission to the furnace reformer, or feeding the converted gas pure carbon dioxide.

Limitation upper limit on CO2in the synthesis gas 10% vol. due to the possibility of reducing the rate of formation of methanol at higher content of carbon dioxide in the gas mixture.

Thus, the essence of the proposed technical solution is the method of producing methanol from the converted mixture of hydrogen and oxides of carbon composition, vol.%: H2- 62,0-78,5; Ar - 0,02-0,07; N2- 0,05-2,2; CH4- 1,0-3,5; CO - 10,4-29,5; CO2- 3,2-10,7 by its contact with the copper-containing catalyst at elevated temperature and pressure in two stages, and the gas mixture of the reformer furnace is divided into two streams in a volume ratio of 100:(1-50), one of which in the first stage, directly in contact with the catalyst in a flow reactor at a temperature of 200-285°C, a pressure of 5-15 MPa and flow rate 800-2000 h-1and the other is mixed with the circulating gas in a volume ratio of 10:(10-100) and with a bulk velocity 2500-10000 h-1sent to the second stage with the release of methanol and water at each stage in the respective devices.

The drawing shows a schematic diagram of the proposed process.

The converted gas from the reforming furnace is udaetsya on the suction side of the compressor 1, cooled air refrigerator 2 and is supplied to the separator 3 for separating moisture. The dried synthesis gas komprimerede to a specified pressure and is divided into two parts. The first (And flow) in contact with the catalyst in a flow reactor 4 and the output from it gives off heat regenerative heat exchanger 5 and the refrigerator-condenser 6. The condensed methanol raw is separated in the separator 7.

In turn, the second part of the converted gas (stream B) is mixed with the circulating gas is heated in the regenerative heat exchanger 8 and is fed to the catalytic reactor horizontal type 9 with built-in heat exchanger 10. Formed etanolsoderjashchaya gas mixture gives off heat reaction of the air to the refrigerator 11 and refrigerator-condenser 12 and is supplied to the separator 7 for separating methanol.

As a catalyst for methanol synthesis using the product in the form of cylindrical pellets with a diameter of 5.2 mm and a height of 5.4 mm, having a composition, wt.%: CuO - 64; ZnO - 24; Al2O3- 10; HgO - 2.

The table below shows examples of the proposed method.

From the description of the invention and the table shows that the claimed technical solution can significantly improve the efficiency of the process, to increase the production of methanol to 82.5 t/h (in the absence of flow reactor is e more than 60 t/h).

The proposed method allows to reduce the amount of catalyst required for processing a given quantity of a gas mixture to reduce energy consumption for circulation of the gas. This opens the way to the creation of methanol units of large capacity without a significant increase in their volume.

Table.
Conditions and results for methanol synthesis according to the examples of its implementation.
IndexThe placeholderExamples
12
The first stage.
The consumption of synthesis gas, thousand

nm3/h
56,07-200,075,3108
Pressure, MPa5,0-8,07,27,1
The average temperature in a flow reactor, °240-260235238
The outlet temperature of the flow reactor, °no data255258
The volume ratio of N2/(CO+CO2in the synthesis gasno data3,22,7
The composition of the synthesis gas, vol.%
CO0.7 to about 30.016,822,0
CO20,2-23,66,6of 5.4
N20,4-3,00,50,7
H2Ono datano
H2no data75,073,3
Arno dataless than 0.05
CH3HEno0,10,05
CH4no datarest
The ratio of CO/CO2(0,03-87):12,54,1
The amount of catalyst, m3About 4-47,620,0
The obtained methanol, t/h1,6-38,8414,8a 21.5
The second stage
Consumption of fresh synthesis gas fed to the second stage, thousand nm3/h44,5-97,325,124,0
The ratio of flows of fresh synthesis gas fed to the first and second stage 3,0:1,04,5:1,0
Reactor pressure, MPa5,0-8,09,8the 10.1
The temperature at the reactor exit, °266-295267270
The amount of circulating gas, thousand nm3/h400-900360400
The volumetric ratio of the converted and the circulation of the gases before mixing-1:14,31:16,7
The ratio of CO/CO2before entering the reactor0,25-555,27,8
The amount of catalyst, m340,0-60,070,0
The obtained methanol, t/h13-40,1155,861,0
Total production of methanol, t/h14,6-78,9570,682,5

A method of producing methanol from the converted mixture of hydrogen and oxides of carbon composition, vol.%: H262,0-78,5; Ar 0,02-0,07; N20,05-2,2; CH41,0-3,5; 10,4-29,5; CO23,2-10,7 by its contact with the copper-containing catalyst at elevated temperature and pressure in two stages, characterized in that the gas mixture of the reformer furnace is divided into two volumetric flow in the ratio of 100:(1-50), one of the first stage directly in contact with the catalyst in a flow reactor at a temperature of 200-285°C, a pressure of 5-15 MPa and flow rate 800-2000 h-1and the other is mixed with the circulating gas in a volume ratio of 10:(10-100) and with a bulk velocity 2500-10000 h-1sent to the second stage, with the separation of methanol and water at each stage in the respective devices.



 

Same patents:

FIELD: chemistry.

SUBSTANCE: invention pertains to the method of methanol obtaining through concentration of a gas mixture, containing carbon oxides and hydrogen, with copper-zinc catalyst at temperature of 200-290°C, pressure of 5-15 MPa, and volume rate of 3000-10000 h-1. The concentrated gas contains the following, in vol %: H2 - 64.0-75.5; Ar - 0.02-0.08; N2 - 0.05-2.0; CH4 - 1.0-3.6; CO - 10.7-19.4; CO2 - 3.3-10.4. The concentrated gas is put into a reformer with volume rate of 800-2000 h-1, mixed with carbon dioxide in volume ratio of (3-100) : 1 and together with cycled gases is passed through 4 catalyst zones of a horizontal reactor at volume ratios of (1.20-1.40):(0.85-0.95):(0.9-1.2):(0.9-1.1), divided by two boilers and one heat exchanger, with cooling of the reaction gas stream and separation of methanol in a separating device.

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FIELD: chemistry.

SUBSTANCE: method includes contact of gas mixture containing carbon oxides and hydrogen ballasted down with nitrogen with copper-containing catalyst under heating, pressure and definite rate velocity of feeding into reactor. Reactor unit consists of two adiabatic-type reactors connected with a pipeline; the original gas mixture containing CO - 10-15 % v/v, CO2 - 0.3-5.0 % v/v, H2 - 15-40 % v/v, N2 -40.0-74.7 % v/v and volumetric ratio H2/(CO+CO2) equal to 1.00-2.91, at 200-260°C and pressure 3.5-5.0 MPa with rate velocity 2000-5000 h-1 is fed into the first reactor with larger main part of unconverted gas fed to circulation and produced at the outlet of the second reactor cooled to 15-20°C and further purified to remove methanol in tower washer and compressed; then the reaction mixture from the first reactor is fed into the second reactor along with the rest minor part of circulating gas indicated above as quench - cold circulation gas fed into the pipeline between the two rectors.

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4 cl, 3 tbl, 1 dwg, 1 exsid1190496

FIELD: industrial organic synthesis.

SUBSTANCE: invention relates to a methanol production process accomplished by contacting gas mixture containing carbon oxides and hydrogen with copper-containing catalyst supplied to a series of at least three flow reactors at specified rate on heating and at pressure while isolating methanol and water from each reactor. Nitrogen-ballasted starting gas mixture is composed of, vol %: CO 10-15, CO2 0.3-5.0, H2 15-40, and N2 40.0-74.7. It is consecutively passed through reactors at volume flow rate 2000-22000 h-1, 200-260°C, pressure 3.5-5.0 MPa, and H2/(CO+CO2) volume ratio 0.75-3.88, while recycling hydrogen separated from tail gases of first and second reactors.

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FIELD: chemical industry; methods and the devices for the heterogeneous synthesis of the chemical compounds.

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FIELD: chemical industry; methods of production of methanol.

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1 tbl, 11 ex, 1 dwg

FIELD: industrial organic synthesis.

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FIELD: chemical industry; installations and the methods of production of the synthesis-gas from the natural gas.

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FIELD: chemical industry; methods of production of hydrogen and a methanol.

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FIELD: industrial organic synthesis and chemical engineering .

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6 cl, 1 dwg, 1 tbl

FIELD: chemistry.

SUBSTANCE: method includes contact of gas mixture containing carbon oxides and hydrogen ballasted down with nitrogen with copper-containing catalyst under heating, pressure and definite rate velocity of feeding into reactor. Reactor unit consists of two adiabatic-type reactors connected with a pipeline; the original gas mixture containing CO - 10-15 % v/v, CO2 - 0.3-5.0 % v/v, H2 - 15-40 % v/v, N2 -40.0-74.7 % v/v and volumetric ratio H2/(CO+CO2) equal to 1.00-2.91, at 200-260°C and pressure 3.5-5.0 MPa with rate velocity 2000-5000 h-1 is fed into the first reactor with larger main part of unconverted gas fed to circulation and produced at the outlet of the second reactor cooled to 15-20°C and further purified to remove methanol in tower washer and compressed; then the reaction mixture from the first reactor is fed into the second reactor along with the rest minor part of circulating gas indicated above as quench - cold circulation gas fed into the pipeline between the two rectors.

EFFECT: method allows increasing methanol yield, efficiency of the process and reducing energy consumption.

4 cl, 3 tbl, 1 dwg, 1 exsid1190496

FIELD: industrial organic synthesis catalysts.

SUBSTANCE: invention relates to copper-containing catalysts for low-temperature synthesis of methanol in fluidized bed at high pressure and provides catalyst, whose preparation involves impregnation and which contains oxides of copper, zinc, chromium, magnesium, aluminum, boron, and barium and has following molar ratio: CuO:ZnO:Cr2O3, MgO:Al2O3:B2O3:BaO = 1:(0.7-1.1):(0.086-0.157):(0.05-0.15):(0.125-0.2):(0.018-0.029):(0.04-0.075).

EFFECT: increased mechanical strength and wear resistance of catalyst.

1 tbl

FIELD: industrial organic synthesis catalysts.

SUBSTANCE: invention relates to copper-containing catalysts for low-temperature synthesis of methanol in fluidized bed at low pressure and provides a wear-resistant catalyst, whose preparation involves impregnation and which contains oxides of copper, zinc, chromium, magnesium, aluminum, and boron and has following molar ratio: CuO:ZnO:Cr2O3, MgO:Al2O3:B2O3 = 1:0.3:(0.15-0.2):(0.1-0.025):(0.25-0.3):(0.08-0.1).

EFFECT: increased mechanical strength and wear resistance of catalyst.

1 tbl

FIELD: industrial organic synthesis catalysts.

SUBSTANCE: invention relates to copper-containing catalysts for low-temperature synthesis of methanol in fluidized bed at median pressure and provides catalyst, whose preparation involves impregnation and which contains oxides of copper, zinc, chromium, magnesium, aluminum, boron, and barium and has following molar ratio: CuO:ZnO:Cr2O3, MgO:Al2O3:B2O3:BaO = 1:0.3:(0.014-0.038):(0.047-0.119):(0.05-0.1):(0.007-0.014):(0.0292-0.054).

EFFECT: increased mechanical strength and wear resistance of catalyst.

1 tbl

The invention relates to a method of producing methanol from natural gas

The invention relates to a method for producing methanol, which finds application in the field of organic synthesis

The invention relates to methods for nizkoatomnye linear alcohols from synthesis gas at pressures not exceeding 100 atmospheres in the presence of a catalyst

FIELD: industrial organic synthesis catalysts.

SUBSTANCE: invention relates to copper-containing catalysts for low-temperature synthesis of methanol in fluidized bed at median pressure and provides catalyst, whose preparation involves impregnation and which contains oxides of copper, zinc, chromium, magnesium, aluminum, boron, and barium and has following molar ratio: CuO:ZnO:Cr2O3, MgO:Al2O3:B2O3:BaO = 1:0.3:(0.014-0.038):(0.047-0.119):(0.05-0.1):(0.007-0.014):(0.0292-0.054).

EFFECT: increased mechanical strength and wear resistance of catalyst.

1 tbl

FIELD: industrial organic synthesis catalysts.

SUBSTANCE: invention relates to copper-containing catalysts for low-temperature synthesis of methanol in fluidized bed at low pressure and provides a wear-resistant catalyst, whose preparation involves impregnation and which contains oxides of copper, zinc, chromium, magnesium, aluminum, and boron and has following molar ratio: CuO:ZnO:Cr2O3, MgO:Al2O3:B2O3 = 1:0.3:(0.15-0.2):(0.1-0.025):(0.25-0.3):(0.08-0.1).

EFFECT: increased mechanical strength and wear resistance of catalyst.

1 tbl

FIELD: industrial organic synthesis catalysts.

SUBSTANCE: invention relates to copper-containing catalysts for low-temperature synthesis of methanol in fluidized bed at high pressure and provides catalyst, whose preparation involves impregnation and which contains oxides of copper, zinc, chromium, magnesium, aluminum, boron, and barium and has following molar ratio: CuO:ZnO:Cr2O3, MgO:Al2O3:B2O3:BaO = 1:(0.7-1.1):(0.086-0.157):(0.05-0.15):(0.125-0.2):(0.018-0.029):(0.04-0.075).

EFFECT: increased mechanical strength and wear resistance of catalyst.

1 tbl

FIELD: chemistry.

SUBSTANCE: method includes contact of gas mixture containing carbon oxides and hydrogen ballasted down with nitrogen with copper-containing catalyst under heating, pressure and definite rate velocity of feeding into reactor. Reactor unit consists of two adiabatic-type reactors connected with a pipeline; the original gas mixture containing CO - 10-15 % v/v, CO2 - 0.3-5.0 % v/v, H2 - 15-40 % v/v, N2 -40.0-74.7 % v/v and volumetric ratio H2/(CO+CO2) equal to 1.00-2.91, at 200-260°C and pressure 3.5-5.0 MPa with rate velocity 2000-5000 h-1 is fed into the first reactor with larger main part of unconverted gas fed to circulation and produced at the outlet of the second reactor cooled to 15-20°C and further purified to remove methanol in tower washer and compressed; then the reaction mixture from the first reactor is fed into the second reactor along with the rest minor part of circulating gas indicated above as quench - cold circulation gas fed into the pipeline between the two rectors.

EFFECT: method allows increasing methanol yield, efficiency of the process and reducing energy consumption.

4 cl, 3 tbl, 1 dwg, 1 exsid1190496

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