The method of producing ammonia with multi-stage pressure increase

 

The invention concerns a method of producing ammonia from synthesis gas. The synthesis of ammonia from fresh synthesis gas containing nitrogen, hydrogen, inert impurities occurs consistently in different synthesis systems, all systems synthesis of respectively one part of the synthesis gas is obtained ammonia and part of it away, and each subsequent synthesis system has a higher pressure than the preceding synthesis system, all system synthesis performed on the basis of fresh gas, the latter synthesis system perform as the circulation and the flow of carrier gas, which lead away from the synthesis system with high blood pressure, after separation and removal of inert components, ammonia, serves as a workflow in the system with lower pressure. The method can reduce the accumulation of inert gases in the circulating system, which allows to reduce the size of hardware synthesis system high pressure at the same power with the installation of only one reaction system. 9 C.p. f-crystals, 4 Il.

The invention concerns a method of producing ammonia NH3under pressure from synthesis gas, which according to reaction (1)

3H2+N2->2N3(1)

contains remethan and inert gases which affect the reaction (1) as to the completeness of its interaction, and hereafter referred to as "inert". Methods of this type are usually arranged so that initially, the fresh synthesis gas multistage compressed to high pressure and then compressed fresh synthesis gas is fed into the cycle, which takes place in one or more reactor filled with a catalyst, in which receive the ammonia. In the circulation process is provided for the separation stage, which received the ammonia is extracted from the cycle in liquid form.

In order to avoid accumulation in the cycle inert, only low concentrations of soluble in the selected ammonia, part fed into the cycle gas is constantly given in the form of a carrier gas. Of the designated carrier gas wash away the remnants of the ammonia and some hydrogen, and in some cases also part of the nitrogen, for example, membrane method or way low-temperature decomposition, allocate and return again in the cycle. The remaining inert, such as methane, argon, helium, and possibly the remaining nitrogen discard or further used to produce heat. The returned gas is admixed to the fresh synthesis gas before compression and thus use again. N is the number of gas separation process undergoes a pressure drop and then these gases with high costs should again be compressed.

For this reason, allow the accumulation of inert gas components from the initial 1-2 vol.% in the fresh synthesis gas to 10-20 vol.% in the circulating gas, although with such high concentrations of inert inevitably associated disadvantage in that the partial pressure of taking part in the reaction gases, which in equilibrium are the only driving force of the reaction is considerably lower than in the synthesis process, free from inert. For this reason, requires a greater consumption of catalyst and a larger volume of the reactor than would be required in the absence of inert.

Despite the described disadvantages associated with the accumulation of inert in the cycle compared to their original content in fresh gas, there is a technical contradiction, which is that when small quantities of carrier gas and thereby a high content of inert production costs, especially the costs of compression, reduced investment costs due to the increased flow of catalyst or the need for more expensive catalysts, for example based on ruthenium, increase. These technical contradiction with the existing prior art insoluble. Therefore, experts re the t optimum cost.

During the synthesis from synthesis gas in a reactor formed a working gas. It consists mainly of unreacted part of the input gas, the formed ammonia and inert. At the outlet of the reactor the resulting ammonia is in gaseous form. To ammonia to separate from the working gas, it is necessary to condense to its liquid form it was possible to deduce from the cycle. Since the dew point of ammonia depends on its partial pressure and temperature, the condensation product is preferably increased pressure of the synthesis process and a high concentration of ammonia, on the one hand, and the low temperature on the other. High concentration of ammonia is achieved by a high consumption of catalyst and low concentration of inert, high pressure synthesis process means, respectively, the energy used to compress the synthesis gas and the low temperature cooling involves the presence of an appropriate cooling equipment for the working gas.

In order to get the ammonia synthesis process using system thermal shift, water or air cooling and/or optionally cyclic cooling can be cool enough to condense and thus could sibiricae relatively high pressure gives the advantage most of the ammonia condenses already at relatively high temperatures that can be achieved by using water cooling (for example, cooling to 30-40C). For example, the dew point at a working concentration of 20 mol.% and the pressure of the synthesis of 200 bar is at approximately 57C. With cooling, for example, up to 35With ammonia in the gas can be reduced to 11.2 mol.%, and receive 59% of the condensation product. Because the working gas which is supplied into the reactor, must contain low concentration of ammonia, in this example of 3.8 mol.%, typically, the cooling system is connected additionally deep cooling to lower temperatures (for example, cooling to a temperature of from -10With 0C) the product has more to condense. Such a system of deep cooling requires energy to reverse the compression evaporating the cooling agent. When the above-described high pressure synthesis, the share of the product, which must be condensed with deep cooling, insignificant and accordingly trebuetsya operating pressure of the synthesis process, as said above, usually in the area of 150-280 bar, and is also known exceptions, in which the pressure in the synthesis process is reduced to 60 bar. The examples described in EP 000993, EP 093502 and EP 179392. Because when the pressure of the synthesis process would have grown disproportionately to the amount of used magmatichnogo catalyst and the associated design requirements for the reactor, these methods based on the use of highly active catalysts. This requires increased consumption magmatichnogo catalyst with the addition of cobalt and ruthenium catalyst due to the presence of a noble metal and therefore more expensive.

The lower the pressure in the synthesis process, the more decreases the amount of heat that can be dissipated using a water or air cooling, and the amount of heat that should be given by deep cooling, respectively, increases. This raises another technical contradiction, which, as a rule, arises from the fact that deep cooling requires cooling system with compressor block. While the cost of compression in the process of synthesis is reduced with a decrease in pressure, the cost of compression in the cooling system is x low pressure, the proportion of condensation before deep cooling increases due to the fact, that is set very low content of inert components in a large flow of carrier gas. The problem with the accumulation of inert occurs as in the synthesis of high pressure, the smaller the content of the inert increases the concentration of the product and thus the dew point. And here the experts are forced to compromise and by evaluating the production and investment costs to find the optimum cost.

For many years obtaining ammonia in krupnoporistogo scale is carried out in a large single units. Odontoclast due to the high cost of the system operating at high pressure in the circulation process, as well as the high cost of the compression process, and both of these factors affected digression was found to increase performance. Therefore, there is a long-term technical bias that economical the obtaining of ammonia is possible only in a single device.

Occasional attempts have been made to this single device to add an additional line, as roughly described in DD 225029. This publication describes two cascaded stages of the synthesis of high pressure at the same pressure level, the first of which is the system with fresh gas, and toulali on such amount, you can get included on the pre-stage fresh gas, and accordingly to reduce the cycle. This system, however, in the last 20 years could not achieve market acceptance, whereupon there was an opinion that only a single installation can be economically viable. The above technical contradictions, however, are related to the reaction systems described in DD 225029.

The present invention therefore is to overcome the above disadvantages and to develop cost-effective method of producing ammonia.

The invention solves the problem that the synthesis of ammonia from synthesis gas occurs consistently in a variety of systems synthesis, and in all of these systems produce ammonia from synthesis gas and a part of him away from there, and each subsequent synthesis system has a higher pressure than the previous one. Under the synthesis system understand the reaction system, which includes a reactor and a device for separating the produced ammonia. Under high pressure thus understand the pressure difference exceeds the pressure loss inside the system synthesis.

In another form of execution of the invention the first synthesis system vypolnim last, executed as of the fresh gas system.

In another form of execution of the invention the last synthesis system is designed as a recirculation system.

In another form of execution of the invention, each system synthesis is separated from the subsequent system of at least one stage of compression.

In another form of execution of the invention, the flow of carrier gas, which is removed from the synthesis system with a higher pressure, after separation and removal of inert components, ammonia and possible other gas components in the form of the original stream is fed into the synthesis system with lower pressure.

The following form of execution of the invention the flow of carrier gas increases so that the enrichment of inert in the system with high pressure is not more than 10 mol.%.

The following form of execution of the invention in at least one reactor fresh gas used catalyst, which contains magnetite with promoters for synthesis of low pressure.

The following form of execution of the invention in at least one reactor fresh gas using a catalyst which contains a noble precious metal and is highly active.

The invention in more detail poyasnee abecause at low pressure, and synthesis system, operating at higher pressure.

Fig.2. The preferred input of the working gas selected from synthesis system operating at low pressure, in the synthesis system, operating at higher pressures in a new installation or upgraded old installation.

Fig.3. The alternate input of the working gas selected from synthesis system operating at low pressure, in the synthesis system, operating at higher pressures in a new installation or upgraded old installation.

Fig.4. Schematic diagram of the layout of several systems of fresh synthesis gas and circulation system synthesis.

For a better understanding of the invention description of the heating system and mechanical connection of the individual compression stages, and their number is omitted.

Fig.1 is that the fresh synthesis gas 1 at the stage of preliminary compression 2 is compressed to a pressure of approximately 60-130 bar, preferably 90-115 bar, because the fresh synthesis gas is not supplied with this pressure usually from upstream installation. This pre-compressed synthesis gas 3 is mixed with the recirculation gas 4. Thus obtained synthesis gas 5 serves first in the first system is and ammonia, which can consist of several separate reactors, cooling and condensing section 8 for condensing the formed ammonia at low temperature and the separator 9 of ammonia to separate the ammonia is condensed from the gas phase, in the form of liquid ammonia 10. Effect of reaction conditions, the synthesis of ammonia in the reactor 7 fresh gas flows, as is known, not fully, and therefore in the reactor 7 fresh gas is used only part of the fresh synthesis gas 1. Residual synthesis gas 11 leaving the separator 9 ammonia is compressed at the stage 12 additional compression to a pressure such that you want to supply it to the second synthesis system 13, which runs at a higher pressure, about 150-280 bar.

The following system 13 synthesis is the synthesis of ammonia in the circulating system according to the prior art, and the resulting ammonia is withdrawn as a liquid product 14. In order to limit the accumulation of inert gas components, continuously drains the wash stream 15. This flushing flow 15 in the enrichment plant 16 first wash ammonia and removing it in the form of liquid ammonia 17, and then separated from the inert gas components and, if necessary, also the nitrogen from gas 4. Instead shown in Fig.1 stage mixing after stage 3 of the provisional compression expedient may be recirculated 19 at the stage of preliminary compression 3 (shown by the dashed line), depending on at what pressure recirculating flow comes from the concentration plant 16. Needless to say, there are simultaneously both types of mixing, for example, when multi-division gas enrichment plant 16. Depending on the design of the enrichment plant 16 along with hydrogen can be regenerated and also nitrogen. The advantage of recycling is that it takes less to produce fresh synthesis gas 1, which is particularly desirable from the standpoint of the energy and construction cost of hydrogen production.

Separated in enrichment plant 16 residual gases consisting mainly of methane and inert gases, may also nitrogen, removed from the process in the form of output stream 18 and can be used energetically and eksergetichesky.

Technical contradictions between the accumulation of inert circulating system for the synthesis of high pressure, on the one hand, and higher costs on the reverse grip, with the other the th installation of 16, can be fully recycled synthesis of low pressure, not requiring re-compression, which is an advantage of the invention. Thus, you can easily efficiently reduce the accumulation of inert circulating system.

A comparison of the existing ammonia synthesis carried out at high pressure, system synthesis high pressure of the same capacity according to the present invention shows that the synthesis system high pressure according to the present invention at the same pressure of the synthesis process can work more efficiently, as due to the lower content of the inert significantly reducing the amount of catalyst increases the partial pressure of ammonia at the outlet of the reactor and thereby moves the dew point of ammonia, thereby reducing the demands cooling agents obtained by condensation of ammonia and by reducing the total amount of circulating gas reduces the cost of transportation, which is an advantage of the invention.

Compared with the traditional process of ammonia synthesis carried out at low pressure, the system for the synthesis of ammonia low pressure according to the present invention has the advantage that it POPs the W inert with fresh gas, even in the case of placing successive systems fresh content of the inert gas from the system to the system increases slowly. Moreover, such equipment can be reduced catalyst or reduced the ratio of high level to the standard catalyst than is usually necessary, which is also an advantage of the invention. For example, can be highly improved magnetite catalysts with promoters for low pressure, and catalysts of noble metals, for example based on ruthenium, be used in smaller quantities. These include nitrides sixth and eighth subgroup of the Periodic system of elements.

Another advantage of the invention is that by dividing the process into several synthesis systems can be implemented by installing a larger capacity size without the shortcomings that arise when replacing a single scheme for multi-line. In the existing methods of obtaining ammonia high pressure, typically require cumbersome installation to compress the synthesis gas and hot devices of the circulation process of high pressure.

In the method according to the invention they all fall away, because the second part of com is that in the system the low pressure unreacted and not skondensiroval. In addition, a smaller content of the inert circulating synthesis process of high pressure reduces the size of the hardware synthesis system high pressure at the same power compared to the setup with only one reaction system. Instead of reducing the size of these favorable properties can be used to increase capacity of existing plants.

Fig.2 shows how the residual synthesis gas after 11 stage 12 compression can be sent to the following system 13 synthesis (depicted by the dashed line), primarily if we are talking about a new installation. This synthesis gas is additionally compressed in stage 12 compression, serves at the point after stage 24 Department of ammonia, but before the reactor 22 of ammonia, as a rule, directly in front of the stage 21 compression, circulation flow, however, it is also possible, in contrast to the scheme shown in Fig.2, the stage 20 of the feed synthesis gas to produce after stage 21 compression of the circulating flow. At the stage 21 of the compression of the circulating flow pressure loss in the individual stages of the method in the circulation system are aligned. After the stage of compression of the circulating flow set the reactor 22 of ammonia, which is usually sostojavshegosa ammonia and separator 24 ammonia, which receive liquid ammonia 14. The outlet 25 of the carrier gas occurs in the largest concentration of inert components at low temperature, which facilitates subsequent separation of the residual portion of the ammonia in the pre-installation 16 (see Fig.1). The remaining circulating gas 26 is directed to stage 20 of the feed synthesis gas, and the cycle.

Fig.3 shows the following input is possible remainder of the synthesis gas after 11 stage 12 additional compression to the second system 13 synthesis (shown by the dashed line), as the new concept of hardware and operating facility, which operates at high pressure. Additionally compressed in stage 12 additional compression of the synthesis gas is injected between the high pressure and the degree of separation of the product. Typically, in existing installations stage 20 of the feed synthesis gas is carried out in or after the cooling and condensing sections 23a or I, however, before the Department 24 of ammonia. In the final stage 21 compression of the circulating flow pressure loss of the individual stages of the method in the circulation system are aligned. After the stage of compression of the circulating flow set the reactor 22 of ammonia, which usually consists of descretely inert. Residual circulation gas 26 is directed to stage 20 of the feed synthesis gas than completing the cycle.

Fig.4 shows a setting in which several systems 27 synthesis presented in the limits indicated by the symbol "n", shaded boxes, and "n" represents any number ranging from 1 sequentially loaded synthesis gas and only the last system 13 synthesis is performed as a closed system. All existing systems 27 synthesis produce ammonia 28. They contain a advanced level 29 compression, and recirculation flows 30 can be at the place mixed with a working synthesis gas.

The invention further more explains two computational examples. The first calculation example shows the installation according to the invention to produce ammonia, contained in the new concept. The second example of the calculation shows the installation according to the invention to produce ammonia in the case of retrofitting existing facility. Since the optimization capabilities of the method depends largely on the relevant related conditions, such as climate, the provision of raw materials, infrastructure, etc., but the specialist may deviate from the suggested as an example of the quantitative proportions, without breaking, however, the idea of the picture is but in Fig.1, the volume flow is given in t/h, the gas concentration in mol.%. Performance is given as the sum of flows 10, 14 and 17 (see table. 2 and 4).

Calculation examples, however, should not be understood so that the greater part of the ammonia is in the last reaction system. Depending on how many set of sequential synthesis systems, it is possible that only a relatively small part of the entire product is made in the last synthesis system.

A list of reference designations

1. Fresh synthesis gas

2. Preliminary compression

3. Pre-compressed synthesis gas

4. The circulating gas

5. Synthesis gas

6. The first synthesis system

7. The fresh gas reactor

8. Cooling and condensing the plot

9. The separator ammonia

10. Liquid ammonia

11. Residual synthesis gas

12. Stage compression

13. Subsequent synthesis system

14. Liquid ammonia

15. The flushing flow

16. Concentration plant

17. Liquid ammonia

18. Output stream

19. Recycling

20. Stage feed synthesis gas

21. Stage seagame the indoor and outdoor areas (split image)

24. The separator ammonia

25. The exhaust gas carrier

26. Circulating gas

27. System synthesis

28. Liquid ammonia

29. Compression stage

30. Recirculation flows

Claims

1. The method of producing ammonia from fresh synthesis gas, which in addition to the reactants, hydrogen and nitrogen contains inert components is carried out in at least two reaction systems, and the synthesis of ammonia from synthesis gas perform consistently in different synthesis systems, and all systems of the synthesis of ammonia is obtained from part of the synthesis gas and part of it away, and each subsequent synthesis system has a higher pressure than the previous synthesis system.

2. The method according to p. 1, characterized in that the first synthesis system perform as the system with fresh gas.

3. The method according to p. 1 or 2, characterized in that all synthesis system, except the last, do as the fresh gas system.

4. The method according to PP.1-3, characterized in that the last synthesis system perform as the circulation system.

5. The method according to PP.1-4, characterized in that each system synthesis is separated from the next by at least one stage of compression.

6. The method according to PP.1-5, characterized in the inert components, ammonia and possibly other gas components, served as a workflow in the system with lower pressure.

7. The method according to p. 6, characterized in that the parameters of the flow of carrier gas is chosen so that the enrichment of inert components in the system with high pressure is not more than 10 mol.%.

8. The method according to PP.1-3, characterized in that at least in the reactor fresh gas used catalyst, which contains magnetite with promoters for low-pressure systems.

9. The method according to PP.1-3, characterized in that at least in the reactor fresh gas used highly active catalyst containing a noble metal.

10. The method according to PP.1-3, characterized in that at least in the reactor fresh gas is used a catalyst containing nitrides sixth and eighth subgroups of the Periodic system of elements.

 

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