CN113460960B - High-concentration carbon monoxide partial conversion process for oxo synthesis - Google Patents
High-concentration carbon monoxide partial conversion process for oxo synthesis Download PDFInfo
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Abstract
The present invention relates to a method forThe invention adopts double bypass control, the flow of the crude synthesis gas shunt is controlled by temperature stabilization, and the water-gas ratio is not required to be regulated by supplementing steam, thus greatly reducing the water-gas ratio of the shift reaction and having remarkable energy-saving effect; the flow of the conversion gas shunt is controlled by adopting the hydrogen-carbon ratio, so that the hydrogen-carbon ratio can be flexibly and effectively regulated, the operation difficulty is reduced, and the CO/H required by a downstream device is accurately regulated 2 Molar ratio; the coarse synthetic gas inlet is provided with the mixer and the low-pressure steam generator, ash and impurities brought by upstream coarse synthetic gas can be effectively condensed along with condensate, a traditional detoxification groove is omitted, the flow is reduced, and the investment is reduced.
Description
Technical Field
The invention relates to a high-concentration carbon monoxide partial conversion process for oxo synthesis.
Background
Currently, in advanced coal gasification processes at home and abroad, an entrained flow process is widely applied industrially, and mainly comprises two major types of coal water slurry gasification and pulverized coal gasification, wherein the pulverized coal gasification is divided into two types of waste boiler type and chilling type due to different cooling modes of high-temperature synthesis gas. Representative waste boiler type processes include Shell pulverized coal gasification technology introduced abroad; the chilling flow comprises a GSP pulverized coal gasification process introduced abroad, a domestic autonomous development 'space furnace', 'eastern furnace' pulverized coal gasification process and the like. The dry volume content of the synthetic gas CO produced by the gasification devices is generally more than 60%, wherein the steam ratio of the chilled pulverized coal gasification synthetic gas is between the traditional high steam ratio and the traditional low steam ratio and is 0.7-1.0, and in the steam ratio range, the high-concentration CO shift reaction is most intense, and the temperature can be more than 500 ℃, so that the reaction temperature can be controlled by reducing the steam ratio, improving the steam ratio or adopting other means.
The low water-gas ratio shift process controls the water-gas ratio of the synthetic gas fed into the first shift converter to be 0.1-0.4 to limit the conversion rate of CO, thereby achieving the purpose of controlling the reaction temperature. However, the risk of methanation reaction is suddenly increased under the conditions of high temperature and low water-gas ratio, the temperature of the shift converter is extremely easy to fly, the catalyst activity is rapidly reduced, the catalyst is frequently replaced, and the long-period stable operation of the device is influenced. For the traditional low water-gas ratio process, the hot spot temperature of the reaction can be reduced, so that the temperature control purpose is achieved; the temperature is controllable and the occurrence of methanation side reaction can be restrained under normal load, but the risk of methanation reaction occurs under the high temperature of the first shift converter under low load working condition or working condition exists.
The high water-gas ratio conversion process aims at preventing the first conversion furnace from overtemperature, and a large amount of superheated steam is added at the inlet of the conversion furnace at one time, so that the water-gas ratio reaches 1.3-1.5 or even higher. For hydrogen production or ammonia synthesis devices, all carbon monoxide in the synthesis gas needs to be converted into hydrogen, so that the reaction depth is large, and the water-gas ratio is usually more than 1.2 to meet the requirements; however, for the oxo synthesis gas (including methanol synthesis, synthetic oil, synthetic natural gas and the like) produced by coal, the total water-gas ratio can meet the requirement of adjusting the hydrogen-carbon ratio without reaching 1.2, so that the additional supplementary steam ensures that the device has high energy consumption and large investment. In addition, for factories with low sulfur content in raw gas, the reverse vulcanization phenomenon can occur due to high temperature and high water-gas ratio, and the sulfur content in the process gas can be maintained by increasing the sulfur content in the process gas by means of high sulfur coal or adding sulfur, so that the selection range of the process is limited.
The catalyst dynamics control process is to control the temperature of the bed layer in a controllable range by reducing the catalyst loading of the first shift converter without adding steam and by a method that the shift reaction does not reach the reaction balance, and the subsequent shift reaction gradually supplements boiler water according to the requirement of the reaction depth, so that steam is basically not needed to be added. However, the method has certain limitation, and the driving force of the reaction is large due to the dual functions of high carbon monoxide content and high water-gas ratio, the equilibrium temperature distance is large, and the dosage of the catalyst must be accurately calculated. If the catalyst loading is out of range, the reaction depth is increased to cause over-temperature; for phases with lower driving load, the crude synthesis gas amount is only half of the normal amount or even lower, and for the same catalyst loading amount, the overtemperature is extremely easy to cause.
Disclosure of Invention
Aiming at the current state of the art, the invention provides a high-concentration carbon monoxide partial conversion process for oxo synthesis, which has the advantages of simple flow, reliable system, small methanation side reaction, small system resistance, good system temperature control, long service life of catalyst and low equipment investment and running cost.
The technical scheme adopted for solving the technical problems is as follows: a high concentration carbon monoxide partial shift process for oxo synthesis comprising the steps of:
spraying a proper amount of mist high-pressure boiler water into the coarse synthesis gas from the upstream through a boiler water regulating valve by a mixer to enable the coarse synthesis gas to form a supersaturated state, then entering a low-pressure steam generator, and obtaining byproduct low-pressure saturated steam, simultaneously reducing the temperature of the coarse synthesis gas to precipitate condensate, settling impurities in the gas along with the condensate, separating the condensate through a gas-liquid separator, entering a coarse synthesis gas heater, and heating to a temperature above the activation temperature point of a catalyst;
the method comprises the steps that crude synthesis gas at an outlet of a crude synthesis gas heater is divided into two parts, one part of crude synthesis gas enters a first conversion furnace, the other part of crude synthesis gas enters a second conversion furnace, dynamic control is adopted in the first conversion furnace, catalyst loading is insufficient, the conversion reaction is not balanced, the conversion gas temperature at the outlet of the reactor is controlled to be 300-450 ℃, and after the conversion gas at the outlet of the first conversion furnace is cooled by a medium-high pressure steam superheater, the conversion gas sequentially passes through the crude synthesis gas heater and a first heat transfer heat exchanger so as to recycle heat energy of the conversion gas step by step;
merging the converted gas and unreacted crude synthesis gas into a second conversion furnace, carrying out thermodynamic equilibrium reaction on the second conversion furnace, cooling the converted gas at the outlet through a second heat transfer heat exchanger, and then entering a subsequent waste heat recovery device.
Preferably, the catalyst bed layer of the first shift converter is arranged in a layered manner, the upper layer is provided with a detoxication agent for removing toxic components such as trace organic sulfur in crude synthesis gas or shift gas, and the lower layer is an axial-radial reactor or an axial reactor.
Preferably, the outlet of the first shift converter is provided with a temperature control structure, and the temperature control structure is linked with a regulating valve which is arranged on the bypass of the first shift converter and can regulate the air inflow of the first shift converter. The adoption of the structure is that: the first shift converter adopts dynamics control, has strict requirements on air inflow, causes the shift converter reaction to tend to be balanced due to less air inflow, has overhigh temperature and is easy to generate methanation reaction, and the problem can be solved after the structure is arranged.
Preferably, after the material output by the first shift converter is subjected to heat energy recovery of shift gas, a second shift converter bypass regulating valve is arranged at the junction with the crude synthetic gas, a hydrogen-carbon ratio control structure is arranged at the downstream of the second shift converter, and the hydrogen-carbon ratio control structure is linked with the second shift converter bypass regulating valve and is used for regulating the shift gas quantity entering the depth shift of the second shift converter according to the final hydrogen-carbon ratio control parameter. The structure is adopted to meet the requirement of the oxo synthesis gas on the hydrogen-carbon ratio, so as to ensure that the hydrogen-carbon ratio is 2.1.
Preferably, the dry carbon monoxide content of the crude synthesis gas from upstream is 30-90% by volume, the water/absolute gas volume ratio is 0.1-1.6, and the pressure is 1.0-9.0 MPaG.
Preferably, the pressure range of the byproduct saturated steam of the low-pressure steam generator is 0.1-2.5 MPaG; the pressure range of the byproduct saturated steam of the medium-high pressure steam generator is 2.5-8.0 MPaG.
Preferably, the raw synthesis gas heater is formed by connecting one or more heat exchangers in series/parallel, and the temperature of the raw synthesis gas outlet is 150-350 ℃.
Preferably, the first heat transfer heat exchanger/the second heat transfer heat exchanger/the waste heat recovery device is formed by connecting one or more heat exchangers in series or in parallel, wherein one side of the waste heat recovery device is cold fluid, and the other side of the waste heat recovery device is hot fluid conversion gas with the outlet temperature of 50-400 ℃.
According to the invention, according to the difference of upstream coarse synthesis gas components and ash and water-gas ratios (if the coarse synthesis gas has low water-gas ratio, the coarse synthesis gas condensate amount in the low-pressure steam generator is small, and the ash removal effect is limited), a detoxification groove is optionally added at the outlet of a raw material gas separator or a coarse synthesis gas heater, so that the ash and toxic components in the coarse synthesis gas can be fully removed. The waste heat recovery device is formed by combining equipment such as a gas-liquid separator, a heat exchanger, a washing tower and the like and is used for recycling, cooling, washing and purifying the waste heat of the converted gas so as to meet the feeding requirement of the downstream acid gas removal device. According to the principle of the utilization of the waste heat of the shift converter, the crude synthetic gas heater in the flow is optionally moved to the outlet of the second shift converter, so that the aim of fully recovering the reaction heat of the shift converter is fulfilled.
Compared with the prior art, the invention has the advantages that: the invention adopts double bypass control, the flow of the crude synthesis gas shunt is controlled by temperature stabilization, and steam is not required to be supplemented to adjust the water-gas ratio, thereby greatly reducing the water-gas ratio of the shift reaction and having obvious energy consumption saving effect; the flow of the conversion gas shunt is controlled by adopting the hydrogen-carbon ratio, so that the hydrogen-carbon ratio can be flexibly and effectively regulatedThe operation difficulty is reduced, and the CO/H required by the downstream device is accurately regulated 2 Molar ratio; the coarse synthetic gas inlet is provided with the mixer and the low-pressure steam generator, ash and impurities brought by upstream coarse synthetic gas can be effectively condensed along with condensate, a traditional detoxification groove is omitted, the flow is reduced, and the investment is reduced.
Drawings
FIG. 1 is a flow chart of embodiment 1 of the present invention;
fig. 2 is a flowchart of embodiment 2 of the present invention.
Detailed Description
The invention is described in further detail below with reference to the embodiments of the drawings.
Example 1:
the high-concentration carbon monoxide partial conversion process for oxo synthesis in this embodiment adopts a reaction system shown in fig. 1, and includes a mixer 1, a boiler water regulating valve 2, a low-pressure steam generator 3, a gas-liquid separator 4, a raw synthesis gas heater 5, a first shift furnace 6, a medium-high pressure steam superheater 7, a first heat transfer heat exchanger 8, a second shift furnace 9, a second heat transfer heat exchanger 10, a waste heat recovery device 11, a first shift furnace bypass regulating valve 12, a temperature control structure 13, a second shift furnace bypass regulating valve 14, and a hydrogen-carbon ratio control structure 15, where the specific connection and coordination relationship of the devices are consistent with those of fig. 1, and detailed description is omitted herein.
The high concentration carbon monoxide partial conversion process for oxo synthesis of the present embodiment comprises the steps of:
spraying a proper amount of mist high-pressure boiler water into the coarse synthesis gas from the upstream through a boiler water regulating valve 2 by a mixer 1 to enable the coarse synthesis gas to form a supersaturated state, then entering a low-pressure steam generator 3, and obtaining byproduct low-pressure saturated steam, simultaneously reducing the temperature of the coarse synthesis gas to precipitate condensate, settling impurities in the gas along with the condensate, separating the condensate through a gas-liquid separator 4, entering a coarse synthesis gas heater 5, and heating to a temperature above the activation temperature point of a catalyst;
the crude synthesis gas at the outlet of the crude synthesis gas heater 5 is divided into two parts, one part of the crude synthesis gas enters the first shift converter 6, the other part of the crude synthesis gas enters the second shift converter 9, wherein the first shift converter 6 adopts dynamic control, the catalyst loading is insufficient, the shift reaction is not balanced, the shift gas temperature at the outlet of the reactor is controlled to be 300-450 ℃, and the shift gas at the outlet of the first shift converter 6 sequentially passes through the crude synthesis gas heater 5 and the first heat transfer heat exchanger 8 after being cooled by the medium-high pressure steam superheater 7 so as to recycle the heat energy of the shift gas step by step;
the converted gas and unreacted crude synthesis gas are converged and enter a second conversion furnace 9, the second conversion furnace 9 adopts thermodynamic equilibrium reaction, and the converted gas at the outlet is cooled by a second heat transfer heat exchanger 10 and then enters a subsequent waste heat recovery device 11.
The catalyst bed layer of the first shift converter 6 is arranged in layers, the upper layer is provided with a detoxication agent for removing toxic components such as trace organic sulfur in crude synthesis gas or shift gas, and the lower layer is an axial-radial reactor or an axial reactor. The outlet of the first shift converter 6 is provided with a temperature control structure 13, and the temperature control structure 13 is linked with a first shift converter bypass regulating valve 12 provided on the bypass of the first shift converter 6 and capable of regulating the intake air amount of the first shift converter 6. The adoption of the structure is that: the first shift converter 6 adopts dynamics control, has strict requirements on air inflow, causes the shift converter reaction to be balanced due to less air inflow, has overhigh temperature and is easy to generate methanation reaction, and the problem can be solved after the structure is arranged.
After the heat energy of the converted gas is recovered from the material output by the first conversion furnace 6, a second conversion furnace bypass regulating valve 14 is arranged at the junction with the crude synthetic gas, a hydrogen-carbon ratio control structure 15 is arranged at the downstream of the second conversion furnace 9, and the hydrogen-carbon ratio control structure 15 is linked with the second conversion furnace bypass regulating valve 14 and is used for regulating the conversion gas quantity entering the second conversion furnace 9 for deep conversion according to the final hydrogen-carbon ratio control parameter. The structure is adopted to meet the requirement of the oxo synthesis gas on the hydrogen-carbon ratio, so as to ensure that the hydrogen-carbon ratio is 2.1.
Example 2:
the high-concentration carbon monoxide partial conversion process for oxo synthesis in this embodiment adopts a reaction system as shown in fig. 2, taking a device for producing methanol by gasification of pulverized coal in a certain chilling flow as an example, and the process in this embodiment specifically includes the following steps:
the crude synthesis gas from the upstream gasification unit has the temperature of 206 ℃, the pressure of 3.84MPaG, the carbon monoxide dry basis content of about 70 percent and the water-gas ratio of 0.92, and is firstly sprayed into a proper amount of mist high-pressure boiler water by a boiler water regulating valve 2 through a mixer 1, then enters a low-pressure steam generator 3, and the byproduct of 0.3MPaG low-pressure saturated steam, and simultaneously the temperature of the crude synthesis gas is reduced to precipitate condensate. And separating condensate by a gas-liquid separator 4, and heating to 230 ℃ by a crude synthesis gas heater 5. The raw synthesis gas at the outlet of the raw synthesis gas heater 5 is divided into two parts: a portion of the raw synthesis gas enters the first shift converter 6 and another portion enters the second shift converter 10. The temperature of the converted gas at the outlet of the first conversion furnace 6 is about 400 ℃, and the converted gas heat is recycled step by step through the medium-high pressure steam superheater 7, the crude synthesis gas heater 5, the first medium-high pressure steam generator 8 and the medium-high pressure boiler water preheater 9 in sequence. The temperature of the converted gas is reduced to 230 ℃, the converted gas and unreacted crude synthesis gas are converged and enter the second conversion furnace 10, and the converted gas at the outlet is cooled by the second medium-high pressure steam generator 11 and then enters the subsequent waste heat recovery device 12. Wherein, the first medium-high pressure steam generator 8 and the second medium-high pressure steam generator 11 both produce medium-high pressure saturated steam of 4.0MPaG as a byproduct, and the saturated steam is sent into a steam pipe network after being overheated by the medium-high pressure steam superheater 7.
The first shift furnace 6 is arranged in layers, the upper layer is provided with detoxication agent, and the lower layer is an axial-radial reactor. Wherein, the lower reactor adopts dynamics control, the catalyst loading is insufficient, and the shift reaction does not reach equilibrium. The temperature control 14 is arranged at the outlet of the first shift converter 6, the air inflow entering the first shift converter 6 is regulated by the first shift converter bypass regulating valve 13, and the temperature of the shift converter 6 outlet is ensured not to exceed 420 ℃.
After heat recovery, the shift gas at the outlet of the water preheater 9 of the medium-high pressure boiler is provided with a second shift furnace bypass regulating valve 15 at the junction with the crude synthetic gas, and the shift gas quantity which enters the second shift furnace 10 for deep shift is regulated according to the final hydrogen-carbon ratio control 16, so that the hydrogen-carbon ratio is ensured to be-2.1, and the final requirement of the synthetic gas product is met.
Claims (5)
1. A high concentration carbon monoxide partial shift process for oxo synthesis comprising the steps of:
spraying a proper amount of mist high-pressure boiler water into the coarse synthesis gas from the upstream through a boiler water regulating valve by a mixer to enable the coarse synthesis gas to form a supersaturated state, then entering a low-pressure steam generator, and obtaining byproduct low-pressure saturated steam, simultaneously reducing the temperature of the coarse synthesis gas to precipitate condensate, settling impurities in the gas along with the condensate, separating the condensate through a gas-liquid separator, entering a coarse synthesis gas heater, and heating to a temperature above the activation temperature point of a catalyst;
the method comprises the steps that crude synthesis gas at an outlet of a crude synthesis gas heater is divided into two parts, one part of crude synthesis gas enters a first conversion furnace, the other part of crude synthesis gas enters a second conversion furnace, dynamic control is adopted in the first conversion furnace, catalyst loading is insufficient, the conversion reaction is not balanced, the conversion gas temperature at the outlet of the reactor is controlled to be 300-450 ℃, and after the conversion gas at the outlet of the first conversion furnace is cooled by a medium-high pressure steam superheater, the conversion gas sequentially passes through the crude synthesis gas heater and a first heat transfer heat exchanger so as to recycle heat energy of the conversion gas step by step;
merging the converted gas and unreacted crude synthesis gas into a second conversion furnace, wherein the second conversion furnace adopts thermodynamic equilibrium reaction, and the converted gas at the outlet enters a subsequent waste heat recovery device after being cooled by a second heat transfer heat exchanger;
the catalyst bed layer of the first shift converter is arranged in layers, the upper layer is provided with a detoxication agent for removing toxic components such as trace organic sulfur in crude synthesis gas or shift gas, and the lower layer is an axial-radial reactor or an axial reactor;
the outlet of the first shift converter is provided with a temperature control structure which is linked with a regulating valve arranged on the bypass of the first shift converter and capable of regulating the air inflow of the first shift converter;
and after the material output by the first shift converter is subjected to shift gas heat energy recovery, a second shift converter bypass regulating valve is arranged at the junction of the material and the crude synthetic gas, a hydrogen-carbon ratio control structure is arranged at the downstream of the second shift converter and is linked with the second shift converter bypass regulating valve, and the shift gas quantity entering the second shift converter for deep shift is regulated according to the final hydrogen-carbon ratio control parameter.
2. The high concentration carbon monoxide partial conversion process for oxo synthesis according to claim 1, wherein: the dry basis volume content of carbon monoxide in the crude synthesis gas from upstream is 30-90%, the volume ratio of water/absolute dry gas is 0.1-1.6, and the pressure range is 1.0-9.0 MPaG.
3. The high concentration carbon monoxide partial conversion process for oxo synthesis according to claim 1, wherein: the pressure range of the byproduct saturated steam of the low-pressure steam generator is 0.1-2.5 MPaG; the pressure range of the byproduct saturated steam of the medium-high pressure steam generator is 2.5-8.0 MPaG.
4. The high concentration carbon monoxide partial conversion process for oxo synthesis according to claim 1, wherein: the crude synthesis gas heater is formed by connecting one or more heat exchangers in series/parallel, and the temperature of the crude synthesis gas outlet is 150-350 ℃.
5. The high concentration carbon monoxide partial conversion process for oxo process according to any one of claims 1 to 4, wherein: the first heat transfer heat exchanger/the second heat transfer heat exchanger/the waste heat recovery device is formed by connecting one or more heat exchangers in series or in parallel, wherein one side of the waste heat recovery device is cold fluid, and the other side of the waste heat recovery device is hot fluid conversion gas with the outlet temperature of 50-400 ℃.
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