A method of producing methanol

 

(57) Abstract:

A method of producing methanol includes a step for synthesis-gas phase Catholic conversion of synthesis gas to methanol in a number of United reactors, including the feeding and heating the synthesis gas in the inlet zone of the reactor by an external carrier, the catalytic conversion of synthesis gas to methanol with heating gas flow due to the heat from the gas stream in the output zone of the reactor, the operation of separating methanol and recycling tail gas. The method differs in that in the inlet zone of the reactor is fed with synthesis gas containing more than 40% vol. nitrogen at a molar ratio of hydrogen to carbon monoxide in the range of 2.8:1 to 1.8:1, the heated gas stream to a temperature of the coolant in the inlet zone of the reactor is carried out with a temperature gradient along the length of the reactor, above the temperature gradient of the heating gas flow in the active portion of the reactor due to the heat of reaction. For example, the process of methanol synthesis is carried out in the temperature range 170 - 280oC, a pressure of 4.0 - 10.0 MPa and volumetric flow rates of 1000 - 10000 h-1the heated gas stream to a temperature of the coolant in the input tonyh reactor is carried out with the second part of the reactor is not more than 3oWith/4 inch C.p. f-crystals, 2 tab., 2 Il.

The invention relates to energy-saving methods for the synthesis of methanol from synthesis gas obtained by partial oxidation of natural gas with air enriched with oxygen, air or the flow of oxygen-containing gas with a high content of nitrogen in the energy machines with electricity generation at all stages of the production of methanol.

More specifically the invention relates to the field of chemical technology, energy-saving processes for the production of methanol from natural gas or "tail" of hydrocarbon gases in the chemical, petrochemical and metallurgical industries.

In the traditional technology of production of methanol is usually the first stage of the process is to obtain synthesis gas steam methane reforming. At this stage is not reached full conversion of methane into synthesis gas and therefore the residual methane is converted at a later stage - steam-oxygen conversion (maybe a combination of these stages). For conducting steam-oxygen conversion is typically used pure oxygen or oxygen-enriched air, the receipt of which is associated with energy costs. There are processes which produced carbon dioxide from synthesis gas. The cost of the produced synthesis gas containing a small amount of nitrogen is high enough that the produced synthesis gas can be used, in addition to the production of methanol in the production of olefin production or motor fuels. The steam reforming reaction of methane vysokoekonomichny and she along with steam-oxygen conversion of methane is carried out in expensive equipment with significant energy and maintenance costs.

The known technology for the production of synthesis gas from natural gas (see Patent US 5.177.114), the cost of which is significantly lower compared to the cost of the synthesis gas obtained by conventional technologies. This is achieved primarily due to the fact that the synthesis gas obtained by partial oxidation of natural gas. Moreover, as the oxidant used is not oxygen, air or air enriched with oxygen. Cost reduction is achieved by:

1) reduce the cost of producing oxygen-enriched air in comparison with the costly production of pure oxygen;

2) use a simpler and less expensive equipment;

3) reduction of operating costs;

4)CSOs process should include the need for the production of synthesis gas, containing significant amounts of nitrogen, up to (40 vol%). Therefore, the production of methanol or motor fuels, or key products of petrochemical synthesis should be carried out on BasicInstallation scheme, otherwise the cost of the target product again would be increased due to the recirculation of large flows of inert components (nitrogen, methane). Thus, the shortcomings of the existing schemes processing of natural gas lie in the complexity of the technological design process, the use of a large number of units of technological equipment, as well as the lack of flexibility of technological schemes for raw materials.

In the German patent DE 4300017 A1 in methanol recycled dilute hydrocarbon gases. However, the low quality of the produced methanol and without the use of heat of chemical reactions and heat of exhaust gases, the cost of the target product will be high, and the installation will not be energotechnology. The latter fact will hinder its use in various industries.

Closest to the claimed method for the production of methanol, selected as a prototype, is the ways the intermediate output generated in reactors of methanol after each catalytic reactor.

The main disadvantage of the invention, taken as a prototype, is the fact that the heat of reaction of partial oxidation of methane and methanol synthesis is not used to generate electricity that can significantly increase the efficiency (and, therefore, reduce the cost of the target product, methanol) industrial installations of this type. In addition, the synthesized methanol contains large amounts of water and organic impurities, which requires to obtain the desired product of high purity rather complicated system of rectification. Therefore, energy consumption for separation also increased compared with the separation of the reaction products that do not contain significant amounts of side components.

Thus, analysis of the known technologies for producing methanol shows that there are no energosensory production of methanol synthesis, which is characterized by obtaining the target product, methanol - high quality.

In the present invention are the following objectives: improving the quality target product, methanol, obtained by reforming of natural gas, and the conversion of heat of chemical reactions at all stages of the chemical is Nola energy, as well as the simplification of the technological scheme of production of methanol, reducing capital and energy costs.

These tasks are solved in the method of producing methanol, comprising the stage of conversion of hydrocarbon feedstocks into synthesis gas-phase catalytic conversion of synthesis gas into methanol in a number of United reactors, including the feeding and heating the synthesis gas in the inlet zone of the reactor by an external carrier, the catalytic conversion of synthesis gas to methanol with heating gas flow due to the heat of reaction of methanol synthesis in the active portion of the reactor, the heat from the gas stream in the output zone of the reactor, the operation of separating methanol and recycling tail gas, in which the input zone of the reactor is fed with synthesis gas, containing more than about 40. % nitrogen at a molar ratio of hydrogen to carbon monoxide in the range from 2.8:1 to 1.8: 1, the heated gas stream to a temperature of the coolant in the inlet zone of the reactor is carried out with a temperature gradient along the length of the reactor, above the temperature gradient of the heating gas flow in the active portion of the reactor due to the heat of reaction.

The difference of the method of producing methanol is that the carbon monoxide in the range from 2.8:1 to 1.8:1, the heated gas stream to a temperature of the coolant in the inlet zone of the reactor is carried out with a temperature gradient along the length of the reactor, above the temperature gradient of the heating gas flow in the active portion of the reactor due to the heat of reaction.

The second variant of the method of producing methanol is characterized by the fact that the process of methanol synthesis is carried out in the temperature range 170-280oC with a pressure of 4.0 to 8.0 MPa and flow rate 500-10000 h-1.

The third variant of the method of producing methanol is characterized by the fact that the heated gas stream to a temperature of the coolant in the inlet zone of the reactor is carried out with a temperature gradient of not more than 10oC/DM, and the temperature gradient of the heating gas flow in the active portion of the reactor is not more than 3oC/inch

The fourth variant of the method of producing methanol is characterized by the fact that the original synthesis gas is divided into two streams, one of which is enriched with hydrogen mass transfer in the membrane installation type and fed to the first catalytic reactor and adjusting the ratio of hydrogen and carbon monoxide, and the second stream depleted in hydrogen, is mixed with the gas stream leaving the last catalyt is Leto combustion of the fuel.

The fifth variant of the method of producing methanol differs in that the vapor produced by the heat of reaction for the synthesis of methanol is fed to the steam turbine to generate electricity and heat tail gases is utilized in gas turbines to generate electricity.

In Fig. 1. illustrates the essence of the invention, which involves the use of a plant producing methanol, comprising three series-connected reactors 1, 2, 3. Each of them has an input zone 4, the main catalytic reaction zone 5, the output zone 6. Weekend zone connected to the separators 7, 8, 9 and they of the heat exchangers 10, 11. At the entrance to the plant (Fig. 1.) posted by compressor 13 and the heat exchanger 12.

In Fig. 2. a schematic energy-saving plant for methanol in accordance with subparagraph. 4, 5 claims. The installation further comprises a membrane unit 14, a steam turbine 15, oven-heated steam and gas flow 16, the gas turbine 17.

An energy-chemical method of producing methanol is implemented with the system shown in Fig. 1,2, as follows.

The feedstock, a synthesis gas with a bulk velocity of 500 - 10000 h-1(received partial is the ora) is supplied to the compressor 13, where compremises, for example, to a pressure of 6.0 MPa. Then he goes into the heat exchanger 12, where it is heated product streams of the 1st reactor to a temperature close to the temperature of the reaction for production of methanol. After the heat exchanger 12 the synthesis gas is fed into the input zone 4 of the reactor 1. It is heated to the temperature of the heating medium with a temperature gradient of not more than 10oC/dm. as the coolant may be, for example, water used. Next, the gas flow passes the zone 5 of the reactor 1, which is the main conversion of synthesis gas to methanol, and zone 6 of the reactor 1. In zone 5 of the reactor 1, the gas stream is heated by the heat of chemical reaction when the temperature gradient along the axis of the reactor, not exceeding 3oC/dm. In zone 6 of the reactor 1 is cooled gas stream and the temperature gradient along the axis of the reactor has a negative value.

From the reactor 1, the gas stream passes the heat exchanger 12, where it heats the feedstock to a temperature close to the temperature in the reactor 1. He then enters the separator 7, where the condensation of methanol, and non-condensable gases pass through the heat exchanger 10 in the input zone 4 reactor 2.

Conditions reactioon 9, where condensed liquid products of the reaction of methanol synthesis, and non-condensable gases are fed into the recovery unit tail gas (shown in Fig. 2).

Option ways, corresponding PP. 4, 5, as follows. Raw synthesis gas with a high content of nitrogen is fed into the compressor, the input of which is fed enriched hydrogen stream of synthesis gas from the membrane unit 14. In membrane apparatus receives a portion of the flow of synthesis gas from the compressor 13. In it, the gas stream is divided into two streams. First - permeate stream enriched in hydrogen, the second - recently stream depleted of hydrogen and enriched with nitrogen.

Komprimierung in the compressor 13-enriched raw hydrogen stream passes through three series-connected reactor to form methanol in each of them (similar to the scheme shown in Fig. 1). Unreacted synthesis gas from the separator 9 is combined with retenti stream and sent to the gas turbine 17 as a gas fuel to generate electricity. Flue gases of the turbine 17 are received in the furnace 16 for heating the steam coming from reactors 1, 2, 3. Superheated 16 steam enters the steam turbine to generate electric is canola.

Therefore, the physico-chemical meaning of the present invention is that the synthesis of methanol is carried out in a nitrogen atmosphere (containing the last more than 40 wt.%) when the set temperature modes of operation of the reactor, providing a highly selective process flow due to the uniformity of heat flows and lack of both in the reactor and the catalyst grain areas with a high content of the reactants.

The invention is illustrated below with specific examples of embodiments of the method.

Example 1. In the energy machine (gas turbine) served 1002 m3/h of methane and the oxidizer (air). The coefficient of excess oxidant 0.35. Formed 5400 m3/h of synthesis gas composition: H2- 27. %, CO is about 1.4. %, N2- 52 about. %, CO2- 3 vol. % 1000 m3clean synthesis gas (without nitrogen) produced more than 0.3 MW of electricity.

The resulting synthesis gas (Fig. 2) is fed to the catalytic reactor 1, in which at a pressure of 6.5 MPa and a temperature of 200oC is synthesized methanol in the amount of 486 kg/h the Reaction mixture at the exit of 1 is cooled in the heat exchanger 12 and the methanol is separated in the separator 7. Neskondensirovannyh the gas flow is heated by the products re>C is synthesized methanol in the amount of 178.2 kg/h composition of the reactants at the inlet 2 is the following: H2- 18.1 about. %. CO - 9.66 about. %, CO2- about 4.0. % Vapour-gas mixture of the reaction products of 2 is cooled in the heat exchanger 10 and the methanol is separated from the reaction products in the separator 8. Non-condensable components of the gas composition: H2- 13.19 about. %, CO - 7.26 about. %, CO2- about 4.5. % after heating in the heat exchanger 11 are received in the catalytic reactor 3, in which at a pressure of 6.5 MPa and a temperature of 210oC is formed 83.2 kg/h of methanol. He after cooling the gas mixture in the heat exchanger 11 is separated in the separator 9.

Total amount of produced methanol - 747.4 kg/h composition of the obtained methanol: water to 1.5 wt.%, methanol - to 98.5 wt.%. The content of other reaction products (dimethyl ether, formate, ethanol) in trace quantities. In catalytic reactors 1, 2, 3 is used, in particular, copper-zinc catalyst type SNM-1.

Catalytic reaction of methanol synthesis in reactors 1, 2, 3 with the amount of catalyst 1150 l each is conducted at the temperature gradients in the input zone of the reactor is less than 10oC/DM and the temperature gradients in the reactor core, less than 3oC/dm. due to heat their chemical reactors is sent to the gas turbine. This produced more than 0.9 MW of electricity.

Example 2. In the energy machine due to partial oxidation 1005 m3/h natural gas is obtained 5400 m3/h of synthesis gas composition: hydrogen - 37.2 about. %, carbon monoxide is about 18.5. %, carbon dioxide - about 3.0. %, methane is about 1.5. %, the rest is nitrogen.

The resulting synthesis gas (total molar flow - 241.07103mol/h) is supplied to the first catalytic reactor. The pressure in the reactor 1 7.0 MPa, a temperature of 220oC. the Molar flow at the exit of 1 is the following: hydrogen - 42.84103mol/h, carbon oxide - 21.18103mol/h of carbon dioxide - 7.13103mol/h, methanol - 23.42103mol/h, inerti - 99.6103mol/H. After cooling and condensation of the gas of methanol and water non-condensable gas components are fed after preheating in heat exchanger 10 in the catalytic reactor 2. The volumetric rate of gas at the entrance to the P-2 3836 m3/h, pressure P-2 - 7.0 MPa, a temperature of 220oC. the Molar flow components at the output of 2 is equal to: hydrogen - 21.80103mol/h, carbon oxide - 10.66103mol/h of carbon dioxide - 6.7103mol/h, inerti - 99.8103mol/H. After cooling, condensation of methanol and water nscontainerframe gases serves the CI gas exit 3: hydrogen - 13.22 103mol/h, carbon oxide - 6.37103mol/h of carbon dioxide - 5.86103mol/h of methanol - 4.29103mol/h, inerti - 100.25103mol/h

Total amount of produced methanol - 1223.2 kg/h, the mass content of water in the liquid reaction products - 2.5 wt.%. In catalytic reactors 1, 2, 3 is used, in particular, copper - zinc catalyst type SNM-1.

All catalytic reactors 1, 2, 3 with the amount of catalyst 1150 l each were carried out with the values of the temperature gradients in the input zone of the reactors 1, 2, 3 less than 10oC/DM, the temperature gradients in the reactor core, 1, 2, 3 less than 3oC/inch

Example 3. In the energy machine is the partial oxidation of 1002 m3/h of natural gas. The composition of the produced synthesis gas: hydrogen - 30.05 about. %, carbon monoxide - 17.41 about. %, carbon dioxide - about 2.03. %, the rest is inert components - nitrogen and methane.

4608 m3/h of synthesis gas are served in catalytic tubular reactor containing 288 tubes. The volume of catalyst in each tube reactor 4 DM3. The pressure in the reaction zone of the reactor 8.0 MPa, a temperature of 220oC. the Amount of liquid reaction products 708,8 L. the methanol Content of EIT temperatures in the reactor core is less than 3oC/dm. In catalytic reactors 1, 2, 3 is used, in particular, copper-zinc catalyst type ICI.

Example 4. In the energy machine is the partial oxidation of 1002 m3/h of natural gas. The composition of the produced synthesis gas: hydrogen - 31.0 about. %, carbon monoxide - 16.2 about. %, carbon dioxide - about 2.03. %, the rest is inert components - nitrogen and methane.

4840 m3/h of synthesis gas are served in catalytic tubular reactor containing 288 tubes. The volume of catalyst in each tube reactor 4 DM3. The pressure in the reaction zone of the reactor 6.5 MPa, temperature 220oC. the Amount of liquid reaction products 662.4 L. the Content of methanol in the catalyzate - 94.5 wt. %, the rest is water. The temperature gradient in the inlet zone of the reactor is less than 10oC/DM, the temperature gradient in the reactor core is less than 3oC/dm. In catalytic reactors 1, 2, 3 is used, in particular, copper-zinc catalyst type ICI.

Example 5. In the energy machine are partial oxidation 1020 m3/h of natural gas. The composition of the produced synthesis gas: hydrogen - 29 about. %, carbon monoxide - 16.0 vol. %, carbon dioxide - about 3.0. %, the rest is inert components - nitrogen and methane. The total molar flow Sol/h, carbon dioxide 7.23103mol/h of the Flow of synthesis gas is sent to the membrane element in which it is divided into permeate and reentry flows. Permeates thread - 4.640 m3/h (molar flows of reactants: hydrogen - 64.2103mol/h, carbon oxide - 29.41103mol/h of carbon dioxide - 6.42103mol/h). Recently thread - 760 m3/h(molar flows of reactants: hydrogen - 5.7103mol/h, carbon oxide - 9.16103mol/h).

Recently stream is directed into the gas turbine, and permeate stream enriched in hydrogen, in a catalytic reactor 1 (Fig. 2). It at a temperature of 205oC, the pressure is 7.0 MPa is formed 489 kg/h of methanol, which is separated in the separator 7 from the gas stream. The molar flows of the components of the synthesis gas into the reactor 2, the following: hydrogen - 33.62103mol/h, carbon oxide - 14.15103mol/h of carbon dioxide - 6.11 103mol/h In the reactor 2 at a pressure of 7.0 MPa, a temperature of 205oC is formed 158.5 kg/h of methanol. After its separation in the separator 8, the synthesis gas is fed into the reactor 3. The molar flows of the reactants entering the reactor 3: hydrogen - 23.72103mol/h, carbon oxide - 9.2103mol/h of carbon dioxide - 6.13103mol/H. it at a pressure of 7.0 MPa, Tg/h

Unreacted synthesis gas is mixed with retenti stream and fed into the gas turbine. In the gas turbine produces over 1.2 MW of electricity.

In catalytic reactors are used, in particular, the catalyst type ICI.

Catalytic reaction of methanol synthesis in reactors 1, 2, 3 with the amount of catalyst 1150 liters each is held at the temperature gradients in the input zone of the reactor is less than 10oC/DM and the temperature gradients in the reactor core, less than 3oC/dm. due to the heat of chemical reactions produced in the steam turbine over 0.07 MW of electricity.

Example 6. In the energy machine is the partial oxidation of 1002 m3/h of natural gas. The composition of the produced synthesis gas: hydrogen - 31.0 about. %, carbon monoxide - 16.2 about. %, carbon dioxide - about 2.03. %, the rest is inert components - nitrogen and methane. The change of temperature modes of the reactor and process indicators are presented in table. 1

Example 7. In the energy machine is the partial oxidation of 1002 m3/h of natural gas. The composition of the produced synthesis gas: hydrogen - 38.1 about. %, carbon monoxide - 18.4 about. %, carbon dioxide - about 2.03. %, the rest is inert components is a Method of producing methanol, including the stage of synthesis gas production, the stage catalytic conversion of synthesis gas into methanol, including the feeding and heating the synthesis gas in the inlet zone of the reactor, the catalytic conversion of synthesis gas to methanol with heating gas flow due to the heat of reaction for methanol synthesis, the allocation of methanol and recycling tail gas, wherein the process is conducted in a number of series-connected reactors, while the heated synthesis gas containing more than 40% vol. nitrogen at a molar ratio of hydrogen to carbon monoxide in the range of 1.8 : 1 to 2.8 : 1 in the input zone of the reactor external coolant until the coolant temperature is the temperature gradient along the length of the reactor, above the temperature gradient of the heating gas flow in the active portion of the reactor due to the heat of the reaction, the dissipation in the output zones of the reactor.

2. A method of producing methanol by p. 1, wherein the methanol synthesis is carried out in the temperature range 170 - 280oC with a pressure of 3.0 to 8.0 MPa, and the volumetric flow rate of 500 to 10000 h-1.

3. A method of producing methanol by PP.1 and 2, characterized in that the heated gas stream to a temperature of the heat is radiant temperature of the heating gas flow in the active portion of the reactor is not more than 3oC/inch

4. A method of producing methanol by PP.1 to 3, characterized in that the raw synthesis gas is divided into two streams, one of which is enriched with hydrogen mass transfer in the membrane installation type and fed to the first catalytic reactor and adjusting the ratio of hydrogen and carbon monoxide, and the second stream depleted in hydrogen, is mixed with the tail gas stream leaving the last catalytic reactor after separation of methanol, and the mixture was fed to utilization in a gas turbine as fuel.

5. A method of producing methanol by PP.1 to 4, characterized in that the recycling tail gas is produced by feeding in a gas turbine power generation.

 

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