CN113460960A - Partial conversion process of high-concentration carbon monoxide for oxo synthesis - Google Patents
Partial conversion process of high-concentration carbon monoxide for oxo synthesis Download PDFInfo
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Abstract
The invention relates to a partial conversion process of high-concentration carbon monoxide for carbonyl synthesis, which adopts double-bypass control, adopts stable temperature control on the flow of a crude synthesis gas shunt circuit, does not need to supplement steam to adjust the water-gas ratio, greatly reduces the water-gas ratio of the conversion reaction, and has obvious energy consumption saving effect; the flow of the variable gas branch is controlled by adopting the hydrogen-carbon ratio, the hydrogen-carbon ratio can be flexibly and effectively adjusted, the operation difficulty is reduced, and the CO/H required by a downstream device is accurately adjusted2A molar ratio; the mixer and the low-pressure steam generator are arranged at the inlet of the crude synthesis gas, so that ash and impurities brought by the upstream crude synthesis 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 partial conversion process of high-concentration carbon monoxide for oxo synthesis.
Background
At present, in advanced coal gasification processes at home and abroad, an entrained flow bed process is widely applied industrially, and mainly comprises two main types of coal water slurry gasification and pulverized coal gasification, wherein the pulverized coal gasification is divided into a waste boiler type and a chilling type due to different cooling modes of high-temperature synthesis gas. A representative waste boiler type process includes a Shell pulverized coal gasification process introduced abroad; the chilling type process comprises a GSP (ground coal gasification) process introduced abroad and a pulverized coal gasification process developed autonomously at home, such as an aerospace furnace and an oriental furnace. The CO dry basis volume content of the synthetic gas produced by the gasification devices is usually up to more than 60%, wherein the water-gas ratio of the chilling type pulverized coal gasification synthetic gas is between the traditional high water-gas ratio and low water-gas ratio and is 0.7-1.0, the high-concentration CO shift reaction is the most severe within the water-gas ratio range, and the temperature can be up to more than 500 ℃, so that the reaction temperature can be controlled by reducing the water-gas ratio, increasing the water-gas ratio or adopting other means.
The low water-gas ratio shift process controls the water-gas ratio of the synthetic gas entering 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 under the conditions of high temperature and low water-gas ratio is increased suddenly, so that the temperature runaway of the shift converter is easy to occur, the activity of the catalyst is reduced rapidly, the catalyst is replaced frequently, and the long-period stable operation of the device is influenced. For the traditional low water-gas ratio process, although the hot spot temperature of the reaction can be reduced, the temperature control purpose is achieved; under normal load, the temperature is controllable and the occurrence of methanation side reaction can be inhibited, but under the working condition of low load or the working condition, the risk of the occurrence of methanation reaction under the high temperature of the first shift converter exists.
The high water-gas ratio conversion process is to prevent 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 to enable the water-gas ratio to reach 1.3-1.5 or even higher. For a hydrogen production or ammonia synthesis device, carbon monoxide in synthesis gas needs to be completely converted into hydrogen, so the reaction depth is large, and the water-gas ratio is usually required to be more than 1.2 to meet the requirement; however, for coal-based oxo gas (including methanol synthesis, synthetic oil, synthetic natural gas and the like), the total water-gas ratio can meet the requirement of adjusting the hydrogen-carbon ratio without reaching 1.2, so that additional steam supplement causes high energy consumption and large investment of the device. In addition, for plants with low sulfur content in the raw material gas, the anti-vulcanization phenomenon occurs due to high temperature and high water-gas ratio, and the sulfur content in the process gas is increased by using high-sulfur coal or adding sulfur, so that normal production can be maintained, and the selection range of the process is limited.
The catalyst dynamics control process is characterized in that the catalyst loading of the first shift converter is reduced, steam does not need to be supplemented, the temperature of a bed layer is controlled within a controllable range by a method that shift reaction does not reach reaction balance, boiler water is gradually supplemented for subsequent shift reaction according to the requirement of reaction depth, and steam does not need to be added basically. However, the method also has certain limitations, and due to the dual functions of high carbon monoxide content and high water-gas ratio, the driving force of the reaction is large, the equilibrium temperature distance is large, and the dosage of the catalyst needs to be accurately calculated. If the catalyst loading exceeds the range, the reaction depth is increased, and the overtemperature is caused; for the stage with lower start-up load, the raw synthesis gas amount is usually only half of the normal amount or even lower, and for the same catalyst loading, the over-temperature is easily caused.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art and provides a partial conversion process of high-concentration carbon monoxide 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 a catalyst, and low equipment investment and operation cost.
The technical scheme adopted by the invention for solving the technical problems is as follows: a partial shift process for high concentration carbon monoxide for oxo synthesis, comprising the steps of:
the method comprises the following steps that (1) crude synthesis gas from upstream is sprayed into appropriate amount of mist high-pressure boiler water through a boiler water regulating valve through a mixer, so that the crude synthesis gas is supersaturated, and then enters a low-pressure steam generator to produce low-pressure saturated steam as a byproduct, meanwhile, the temperature of the crude synthesis gas is reduced to separate out condensate, impurities in the gas are precipitated along with the condensate, the condensate is separated out through a gas-liquid separator, and the condensate enters a crude synthesis gas heater and is heated to a temperature above a catalyst activation temperature point;
the method comprises the following steps that the raw synthesis gas at the outlet of a raw synthesis gas heater is divided into two parts, one part of the raw synthesis gas enters a first shift converter, the other part of the raw synthesis gas enters a second shift converter, the first shift converter is dynamically controlled, the loading amount of a catalyst is insufficient, the shift reaction is not balanced, the temperature of shift gas at the outlet of the reactor is controlled to be 300-450 ℃, the shift gas at the outlet of the first shift converter is cooled by a medium-high pressure steam superheater and then sequentially passes through the raw synthesis gas heater and a first heat transfer heat exchanger, so that the heat energy of the shift gas is recycled step by step;
and converging the converted gas and the 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.
Preferably, the catalyst bed layer of the first shift converter is arranged in a layered mode, the upper layer is provided with a detoxifying agent for removing trace toxic components such as organic sulfur and the like in the crude synthesis gas or the 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 which is linked with a regulating valve which is arranged on the first shift converter bypass and can regulate the air inflow of the first shift converter. Adopt above-mentioned structure, because: the first shift converter adopts dynamic control, has strict requirements on air inflow, and the air inflow is less, so that the shift converter tends to balance in reaction, the temperature is too high, and methanation reaction is easy to occur.
Preferably, after the heat energy of the converted gas is recovered, a second converter bypass regulating valve is arranged at the junction of the material output by the first converter and the crude synthesis gas, and a hydrogen-carbon ratio control structure is arranged at the downstream of the second converter and is linked with the second converter bypass regulating valve for regulating the converted gas amount entering the second converter for deep conversion according to the final hydrogen-carbon ratio control parameter. By adopting the structure, the requirement of the carbonyl synthesis gas on the hydrogen-carbon ratio is met, and the hydrogen-carbon ratio is ensured to be 2.1.
Preferably, the volume content of carbon monoxide dry basis in the raw synthesis gas from upstream is 30-90%, the volume ratio of water to absolute dry gas is 0.1-1.6, and the pressure range is 1.0-9.0 MPaG.
Preferably, the byproduct saturated steam pressure of the low-pressure steam generator ranges from 0.1 MPaG to 2.5 MPaG; the byproduct saturated steam pressure range 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/in parallel, and the outlet temperature of the raw synthesis gas 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 provided with cold fluid, and the other side of the waste heat recovery device is provided with hot fluid change gas with the outlet temperature of 50-400 ℃.
According to the invention, according to the difference of upstream raw synthesis gas components and the ratio of ash to water to gas (if the ratio of water to gas of the raw synthesis gas is low, the amount of condensed liquid of the raw synthesis gas in the low-pressure steam generator is small, and the effect of removing ash is limited), a detoxification groove is optionally added at the outlet of the raw gas separator or the heater of the raw synthesis gas to ensure that the ash and toxic components in the raw 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 transformed gas so as to meet the feeding requirement of a downstream acid gas removal device. According to the principle of utilization of the waste heat of the shift conversion gas, the crude synthesis gas heater in the process can be selectively moved to the outlet of the second shift conversion furnace, so that the purpose of fully recovering the reaction heat of the shift conversion furnace is achieved.
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 stably controlled by temperature, and steam is not needed to be supplemented to adjust the water-gas ratio, so that the water-gas ratio of the shift reaction is greatly reduced, and the energy consumption saving effect is obvious; the flow of the variable gas branch is controlled by adopting the hydrogen-carbon ratio, the hydrogen-carbon ratio can be flexibly and effectively adjusted, the operation difficulty is reduced, and the CO/H required by a downstream device is accurately adjusted2A molar ratio; the mixer and the low-pressure steam generator are arranged at the inlet of the crude synthesis gas, so that ash and impurities brought by the upstream crude synthesis 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 flowchart of example 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 accompanying examples.
Example 1:
the partial shift conversion process of high concentration carbon monoxide for oxo synthesis in the embodiment adopts a reaction system as 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 converter 6, a medium-high pressure steam superheater 7, a first heat transfer heat exchanger 8, a second shift converter 9, a second heat transfer heat exchanger 10, a waste heat recovery device 11, a first shift converter bypass regulating valve 12, a temperature control structure 13, a second shift converter bypass regulating valve 14, and a hydrogen-carbon ratio control structure 15, and specific connections and matching relations of the devices conform to those in fig. 1, which are not described herein.
The high concentration carbon monoxide partial shift process for oxo of this example comprises the following steps:
the method comprises the following steps that (1) crude synthesis gas from upstream is sprayed into a proper amount of mist high-pressure boiler water through a boiler water regulating valve 2 through a mixer 1, so that the crude synthesis gas is supersaturated, then enters a low-pressure steam generator 3, low-pressure saturated steam is produced as a byproduct, meanwhile, the temperature of the crude synthesis gas is reduced, condensate is separated out, impurities in the gas settle with the condensate, the condensate is separated out through a gas-liquid separator 4, and the condensate enters a crude synthesis gas heater 5 and is heated to a temperature above the activation temperature point of a catalyst;
the method comprises the following steps that the raw synthesis gas at the outlet of a raw synthesis gas heater 5 is divided into two parts, one part of the raw synthesis gas enters a first shift converter 6, the other part of the raw synthesis gas enters a second shift converter 9, wherein the first shift converter 6 is dynamically controlled, the loading amount of a catalyst is insufficient, the shift reaction is not balanced, the temperature of shift gas at the outlet of a reactor is controlled to be 300-450 ℃, and the shift gas at the outlet of the first shift converter 6 is cooled through a medium-high pressure steam superheater 7 and then sequentially passes through the raw synthesis gas heater 5 and a first heat transfer heat exchanger 8 so as to recycle the heat energy of the shift gas step by step;
the converted gas and the unreacted crude synthesis gas are converged and enter a second shift converter 9, the second shift converter 9 adopts thermodynamic equilibrium reaction, and the converted gas at the outlet enters a subsequent waste heat recovery device 11 after being cooled by a second heat transfer heat exchanger 10.
The catalyst bed layer of the first shift converter 6 is arranged in layers, the upper layer is provided with a detoxifying agent for removing trace toxic components such as organic sulfur in the 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 mechanism 13, and the temperature control mechanism 13 is linked with a first shift converter bypass regulating valve 12 provided in a bypass of the first shift converter 6 and capable of regulating the intake air amount of the first shift converter 6. Adopt above-mentioned structure, because: the first shift converter 6 adopts dynamic control, has strict requirements on air inflow, and the shift converter tends to be balanced due to less air inflow, has overhigh temperature and is easy to generate methanation reaction.
After the heat energy of the converted gas of the material output by the first conversion furnace 6 is recovered, a second conversion furnace bypass regulating valve 14 is arranged at the junction of the material and the crude synthesis 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 used for regulating the converted gas amount entering the second conversion furnace 9 for deep conversion according to the final hydrogen-carbon ratio control parameter. By adopting the structure, the requirement of the carbonyl synthesis gas on the hydrogen-carbon ratio is met, and the hydrogen-carbon ratio is ensured to be 2.1.
Example 2:
the partial shift process of high concentration carbon monoxide 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 chilling process as an example, the process in this embodiment specifically includes the following steps:
the raw synthesis gas from an upstream gasification unit is sprayed with a proper amount of atomized high-pressure boiler water under the control of a boiler water regulating valve 2 through a mixer 1 at the temperature of 206 ℃, the pressure of 3.84MPaG, the dry basis content of carbon monoxide of about 70 percent and the water-gas ratio of 0.92, and then enters a low-pressure steam generator 3 to produce a byproduct of 0.3MPaG low-pressure saturated steam, and the temperature of the raw synthesis gas is reduced to separate out condensate. And then the condensate is separated by a gas-liquid separator 4 and enters a crude synthesis gas heater 5 to be heated to 230 ℃. The raw synthesis gas at the outlet of the raw synthesis gas heater 5 is divided into two parts: a part of the raw synthesis gas enters a first shift converter 6, and the other part of the raw synthesis gas enters a 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 passes through a medium-high pressure steam superheater 7, a crude synthesis gas heater 5, a first medium-high pressure steam generator 8 and a medium-high pressure boiler water preheater 9 in sequence to recycle the heat of the converted gas step by step. The temperature of the converted gas is reduced to 230 ℃, the converted gas and the unreacted crude synthesis gas are converged and enter a second shift converter 10, and the converted gas at the outlet is cooled by a second medium-high pressure steam generator 11 and then enters a subsequent waste heat recovery device 12. Wherein, the first middle-high pressure steam generator 8 and the second middle-high pressure steam generator 11 both produce middle-high pressure saturated steam of 4.0MPaG, and are sent into a steam pipe network after being superheated by the middle-high pressure steam superheater 7.
The first shift converter 6 is arranged in layers, the upper layer is provided with a detoxifying agent, and the lower layer is an axial-radial reactor. Wherein, the lower reactor adopts dynamic control, the catalyst loading is not enough, and the shift reaction does not reach balance. The outlet of the first shift converter 6 is provided with a temperature control 14, and the air inlet amount entering the first shift converter 6 is adjusted through a first shift converter bypass adjusting valve 13, so that the temperature of the shift air at the outlet of the first shift converter 6 is ensured not to exceed 420 ℃.
After heat recovery, the transformed gas at the outlet of the medium-high pressure boiler water preheater 9 is provided with a second shift converter bypass regulating valve 15 at the junction with the crude synthesis gas, the transformed gas amount entering the second shift converter 10 for deep conversion is regulated according to a final hydrogen-carbon ratio control 16, and the hydrogen-carbon ratio is ensured to be-2.1 so as to meet the final requirement of a synthesis gas product.
Claims (8)
1. A partial shift process for high concentration carbon monoxide for oxo synthesis, comprising the steps of:
the method comprises the following steps that (1) crude synthesis gas from upstream is sprayed into appropriate amount of mist high-pressure boiler water through a boiler water regulating valve through a mixer, so that the crude synthesis gas is supersaturated, and then enters a low-pressure steam generator to produce low-pressure saturated steam as a byproduct, meanwhile, the temperature of the crude synthesis gas is reduced to separate out condensate, impurities in the gas are precipitated along with the condensate, the condensate is separated out through a gas-liquid separator, and the condensate enters a crude synthesis gas heater and is heated to a temperature above a catalyst activation temperature point;
the method comprises the following steps that the raw synthesis gas at the outlet of a raw synthesis gas heater is divided into two parts, one part of the raw synthesis gas enters a first shift converter, the other part of the raw synthesis gas enters a second shift converter, the first shift converter is dynamically controlled, the loading amount of a catalyst is insufficient, the shift reaction is not balanced, the temperature of shift gas at the outlet of the reactor is controlled to be 300-450 ℃, the shift gas at the outlet of the first shift converter is cooled by a medium-high pressure steam superheater and then sequentially passes through the raw synthesis gas heater and a first heat transfer heat exchanger, so that the heat energy of the shift gas is recycled step by step;
and converging the converted gas and the 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.
2. The high concentration carbon monoxide partial shift process for oxo synthesis according to claim 1, wherein: the catalyst bed layer of the first shift converter is arranged in a layered mode, the upper layer is provided with a detoxifying agent and used for removing trace toxic components such as organic sulfur and the like in the crude synthesis gas or the shift gas, and the lower layer is an axial-radial reactor or an axial reactor.
3. The high concentration carbon monoxide partial shift process for oxo synthesis according to claim 1, wherein: the outlet of the first shift converter is provided with a temperature control structure which is linked with a regulating valve which is arranged on a bypass of the first shift converter and can regulate the air input of the first shift converter.
4. The high concentration carbon monoxide partial shift process for oxo synthesis according to claim 1, wherein: and after the heat energy of the converted gas of the material output by the first conversion furnace is recovered, a second conversion furnace bypass regulating valve is arranged at the junction of the material and the crude synthesis gas, and a hydrogen-carbon ratio control structure is arranged at the downstream of the second conversion furnace and is linked with the second conversion furnace bypass regulating valve and used for regulating the converted gas amount entering the second conversion furnace for deep conversion according to the final hydrogen-carbon ratio control parameter.
5. The high concentration carbon monoxide partial shift process for oxo according to any one of claims 1 to 4, wherein: the volume content of carbon monoxide dry basis in the crude synthesis gas from upstream is 30-90%, the volume ratio of water to absolute dry gas is 0.1-1.6, and the pressure range is 1.0-9.0 MPaG.
6. The high concentration carbon monoxide partial shift process for oxo according to any one of claims 1 to 4, wherein: the byproduct saturated steam pressure range of the low-pressure steam generator is 0.1-2.5 MPaG; the byproduct saturated steam pressure range of the medium-high pressure steam generator is 2.5-8.0 MPaG.
7. The high concentration carbon monoxide partial shift process for oxo according to any one of claims 1 to 4, wherein: the raw synthesis gas heater is formed by connecting one or more heat exchangers in series/in parallel, and the outlet temperature of the raw synthesis gas is 150-350 ℃.
8. The high concentration carbon monoxide partial shift process for oxo 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 provided with cold fluid, and the other side of the waste heat recovery device is provided with hot fluid change gas with the outlet temperature of 50-400 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011034855A2 (en) * | 2009-09-18 | 2011-03-24 | Hydrogen Energy International Limited | Processes and apparatuses for reducing pollutants and producing syngas |
| CN102442643A (en) * | 2011-09-27 | 2012-05-09 | 中国寰球工程公司 | High-concentration carbon monoxide transformation process with low steam consumption |
| CN110550602A (en) * | 2019-08-08 | 2019-12-10 | 中石化宁波工程有限公司 | controllable semi-isothermal conversion process for high-concentration carbon monoxide for oxo synthesis |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011034855A2 (en) * | 2009-09-18 | 2011-03-24 | Hydrogen Energy International Limited | Processes and apparatuses for reducing pollutants and producing syngas |
| CN102442643A (en) * | 2011-09-27 | 2012-05-09 | 中国寰球工程公司 | High-concentration carbon monoxide transformation process with low steam consumption |
| CN110550602A (en) * | 2019-08-08 | 2019-12-10 | 中石化宁波工程有限公司 | controllable semi-isothermal conversion process for high-concentration carbon monoxide for oxo synthesis |
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