CN110921615A - Method for preparing ammonia product by combining high-pressure coal water slurry radiation waste boiler type gasification with low-pressure ammonia synthesis - Google Patents
Method for preparing ammonia product by combining high-pressure coal water slurry radiation waste boiler type gasification with low-pressure ammonia synthesis Download PDFInfo
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- CN110921615A CN110921615A CN201911236722.6A CN201911236722A CN110921615A CN 110921615 A CN110921615 A CN 110921615A CN 201911236722 A CN201911236722 A CN 201911236722A CN 110921615 A CN110921615 A CN 110921615A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/025—Preparation or purification of gas mixtures for ammonia synthesis
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/04—Preparation of ammonia by synthesis in the gas phase
- C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
- C01C1/0411—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst characterised by the catalyst
Abstract
The embodiment of the invention discloses a method for preparing ammonia products by combining high-pressure coal water slurry radiation waste boiler type gasification with low-pressure ammonia synthesis, and belongs to the technical field of synthetic ammonia production by coal water slurry. The method comprises a boiler unit, a coal water slurry preparation unit, a high-pressure coal water slurry radiation waste boiler type gasification unit, a transformation unit, a low-temperature methanol washing unit, a liquid nitrogen washing unit and a low-pressure ammonia synthesis unit. The method solves the problems of longer process, large occupied area, high operating pressure, high investment, large danger coefficient and high production cost in the prior art.
Description
Technical Field
The embodiment of the invention relates to the technical field of synthetic ammonia production by coal water slurry, in particular to a method for preparing an ammonia product by combining high-pressure coal water slurry radiation waste boiler type gasification with low-pressure ammonia synthesis.
Background
Currently, the production of synthetic ammonia from coal is becoming mainstream, wherein the technical route of preparing synthesis gas by using a coal water slurry pressure gasification technology has already occupied most of the proportion in the field of ammonia synthesis due to the advantages of cleanness, high efficiency, safety, easiness in large-scale production and the like. The technical route mainly comprises the following steps: oxygen obtained by separation of an air separation unit and coal water slurry are subjected to complex oxidation-reduction reaction (the reaction pressure is about 6.5 MPa) in a combustion chamber of a gasification furnace, and CO and H are discharged after washing and cooling2、CO2、CH4、H2The synthesis method comprises the following steps of (1) raw synthesis gas (the pressure is about 6.3 MPa) with S as a main component, sequentially converting carbon monoxide in the raw synthesis gas into hydrogen through a conversion unit (the pressure of discharged conversion gas is about 6.0 MPa), removing carbon dioxide and hydrogen sulfide through a low-temperature methanol washing unit (the pressure of discharged purified gas is about 5.8 MPa), removing a small amount of carbon monoxide and methane through a liquid nitrogen washing unit to obtain hydrogen (the pressure is about 5.7 MPa), then pressurizing the hydrogen and the nitrogen separated from an air separation unit according to a certain molar ratio through a compression unit, sending the nitrogen into an ammonia synthesis unit (the reaction pressure is 13-15 MPa), cooling the synthesized ammonia at high temperature and high pressure under the action of a catalyst, and then conveying the cooled ammonia to a liquid ammonia tank for storage. The specific process flow refers to fig. 1.
The process has the following disadvantages: (1) at present, the pressurized gasification of the coal water slurry basically adopts a chilling process, namely 1300-1500 ℃ high-temperature gas discharged from a combustion chamber of a gasification furnace is directly chilled by chilling water, and high-level heat energy is not reasonably recycled, so that energy waste is caused. (2) The ammonia synthesis tower has high operation pressure, nitrogen and hydrogen generally react under 13-15 MPa, the pressure of the converted and washed crude synthesis gas is generally about 5.7MPa, and after the crude synthesis gas is mixed and matched with the nitrogen, a compressor is needed for pressurization, so that the overall energy consumption is high, and more potential safety hazards exist.
In view of the problems of longer flow, large occupied area, high operating pressure, large danger coefficient, high production cost and high investment in the prior art, the prior water-coal-slurry pressure gasification technology needs to be improved.
Disclosure of Invention
Therefore, the embodiment of the invention provides a method for preparing an ammonia product by combining high-pressure coal water slurry radiation waste boiler type gasification with low-pressure ammonia synthesis, which aims to solve the problems of longer flow, large floor area, high operating pressure, high investment risk, large risk factor and high production cost in the prior art.
In order to achieve the above object, the embodiments of the present invention provide the following technical solutions:
a method for preparing ammonia products by combining high-pressure coal water slurry radiation waste boiler type gasification with low-pressure ammonia synthesis, which comprises the following steps:
1) superheated steam generated by the boiler unit provides driving power for the air separation unit, and air is separated into at least oxygen and nitrogen by adopting a low-temperature separation technology;
2) the oxygen is used as a gasifying agent and is subjected to gasification reaction with the coal water slurry prepared by the coal water slurry preparation unit in a high-pressure coal water slurry radiation waste boiler type gasification unit and heat exchange to obtain crude synthesis gas and by-product high-pressure steam;
3) the crude synthesis gas is conveyed to a conversion unit, carbon monoxide in the crude synthesis gas is converted into hydrogen to obtain conversion gas, and medium-pressure saturated steam and low-pressure saturated steam are produced as byproducts;
4) the converted gas is conveyed to a low-temperature methanol washing unit, and at least hydrogen sulfide and carbon dioxide in the converted gas are removed to obtain purified gas;
5) the purified gas is sent to a liquid nitrogen scrubbing unit to remove at least a small amount of carbon monoxide and methane from the purified gas to obtain CO and CO2A hydrogen product having a content of less than 10 PPm;
6) and (3) directly conveying the nitrogen obtained by the separation in the step (1) and the hydrogen product obtained in the step (5) to a low-pressure ammonia synthesis unit, carrying out ammonia synthesis reaction under the action of ZA-5 type catalyst, and cooling the generated ammonia gas to obtain liquid ammonia.
In a preferred embodiment, in the step 2, the reaction pressure of a combustion chamber of a gasification furnace of the coal water slurry radiation waste boiler type gasification unit is 8.0-8.7 MPa, and the byproduct of saturated steam with the pressure higher than 9.0MPa is generated.
In a preferred embodiment, in the step 2, the pressure of the obtained raw synthesis gas is 7.8-8.5 MPa.
In a preferred embodiment, in the step 3, the pressure of the converted gas is 7.6-8.3 MPa.
In a preferred embodiment, in the step 4, the pressure of the purified gas obtained is 7.5-8.2 MPa.
In a preferred embodiment, in the step 6, the feeding molar ratio of the hydrogen product to the nitrogen is 2.0-2.5, the reaction pressure is 7.2-8.0 MPa, and the maximum reaction temperature is not more than 460 ℃.
In a preferred embodiment, in step 2, the high-pressure steam output by the high-pressure coal water slurry radiation waste boiler type gasification unit is preheated and then is changed into superheated power steam which can be used for providing driving power for the air separation unit.
In a preferred embodiment, in step 6, the purge gas discharged from the low pressure ammonia synthesis unit is pressurized and returned to the low pressure ammonia synthesis column.
The embodiment of the invention has the following advantages:
1. the invention adopts ZA-5 type ammonia synthesis catalyst, reduces the synthesis pressure to 7.2-8.0 MPa, reduces the energy consumption and reduces the synthesis purge gas amount.
2. The invention adopts 8.0-8.7 MPa water-coal-slurry radiation waste boiler type gasification technology to replace a gasifier chilled water system, obtains high-grade high-pressure steam as a byproduct, and improves the energy recovery utilization rate.
3. The pressure of the mixed gas of the hydrogen discharged from the liquid nitrogen washing unit and the nitrogen separated by the air separation unit is 7.2-8.0 MPa, and the mixed gas is directly conveyed to the low-pressure ammonia synthesis tower for reaction without being pressurized by a compressor, so that the production flow is simplified, the energy consumption is reduced, and the direct investment is reduced.
4. The invention takes the organic sewage which is generated by each unit and is difficult to treat as the water for preparing the coal water slurry, thereby saving the sewage treatment cost and avoiding the environmental pollution.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.
FIG. 1 is a flow chart of a conventional method for preparing ammonia products by pressure gasification of coal water slurry;
FIG. 2 is a flow chart of a method for preparing ammonia products by combining high-pressure water-coal-slurry radiation waste boiler type gasification and low-pressure ammonia synthesis provided by the embodiment of the invention.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Examples
FIG. 2 is a flow chart of a method for preparing ammonia products by combining high-pressure coal water slurry radiation waste boiler type gasification with low-pressure ammonia synthesis. The method comprises the following steps:
and the boiler unit is used for heating the working medium by utilizing the heat emitted by fuel combustion to produce superheated steam with certain pressure and temperature, and the produced superheated steam is used for providing driving power for a compressor unit of the air separation unit. Boiler coal is generally used as fuel.
The air separation unit adopts low-temperature separation technology such as low-temperature rectification to separate air into oxygen, nitrogen, argon and the like, the oxygen is used as a gasification agent and is conveyed to the high-pressure coal slurry radiation waste boiler type gasification unit, the nitrogen is used as a reaction raw material and is conveyed to the low-pressure ammonia synthesis unit, and meanwhile, the nitrogen is used as replacement gas and protective gas to be recycled for other units in the whole plant. The argon can be directly sold as product gas.
The coal water slurry preparation unit is prepared by raw material coal and organic sewage according to a certain proportion, and preferably, the coal water slurry preparation unit also comprises a pH regulator or fluxing agent limestone and the like. The organic sewage is derived from organic waste liquid or low-salt wastewater which is generated by each unit and is difficult to treat, and is used as water for preparing coal water slurry, so that the sewage treatment cost is saved, and the environmental pollution is avoided.
The high pressure water-coal slurry radiation waste boiler type gasification unit comprises a gasification furnace combustion chamber, a radiation waste boiler, a chilling chamber and a gas washing tower. Oxygen obtained by separation of the air separation unit and the coal water slurry prepared by the coal water slurry preparation unit are conveyed to a gasification furnace combustion chamber through a nozzle to carry out gasification reaction, the reaction pressure of the gasification furnace combustion chamber is 8.0-8.7 MPa, preferably, the reaction pressure is 8.5MPa, high-temperature crude synthesis gas (the temperature is 1300-1500 ℃) discharged from the gasification furnace combustion chamber is subjected to heat exchange and cooling through a radiation waste boiler, a chilling chamber and a gas washing tower, the cooled crude synthesis gas (the pressure is 7.8-8.5 MPa) is conveyed to a conversion unit, water in the waste boiler absorbs heat and then becomes high-grade high-pressure steam, and the high-grade high-pressure steam can be directly merged into an enterprise steam pipe network, can also be used for power generation, and other purposes. Preferably, the high-pressure steam can be superheated and used for providing driving power for a compressor unit of the air separation unit.
And the conversion unit is used for converting carbon monoxide in the crude synthesis gas discharged by the high-pressure water-coal-slurry radiation waste boiler type gasification unit into hydrogen required by the ammonia synthesis reaction by utilizing the reaction of the carbon monoxide and water vapor, and simultaneously by-products of medium-pressure saturated steam and low-pressure saturated steam are generated. The pressure of the conversion gas discharged by the conversion unit is 7.6-8.3 MPa, preferably 8.3MPa, the pressure of the medium-pressure saturated steam is 5.0-8.5 MPa, and the pressure of the low-pressure saturated steam is 0.5-2.5 MPa.
The low-temperature methanol washing unit removes gases such as hydrogen sulfide and carbon dioxide in the conversion gas output by the conversion unit by utilizing the characteristic that methanol has high solubility to acid gas at low temperature and selectively absorbs the acid gas, and the pressure of the discharged purified gas is 7.5-8.2 MPa, preferably 8.1 MPa.
And the sulfur recovery unit is used for recycling the hydrogen sulfide removed by the low-temperature methanol washing unit, for example, preparing sulfur or sulfuric acid products.
A liquid nitrogen washing unit for washing off a small amount of carbon monoxide and methane contained in the purified gas discharged from the low-temperature methanol washing unit by using liquid nitrogen under a low-temperature condition to obtain CO and CO2Hydrogen product with a content of less than 10 PPm.
And the synthetic ammonia unit is used for directly conveying the hydrogen product discharged by the liquid nitrogen washing unit and nitrogen obtained by separating the air separation unit to a low-pressure ammonia synthesis tower (the reaction pressure is 7.2-8.0 MPa), carrying out ammonia synthesis reaction under the action of ZA-5 type catalyst, conveying the generated ammonia gas to an ammonia cooler for separation, and conveying the produced liquid ammonia as a product to a liquid ammonia tank for storage.
Specifically, the method for preparing ammonia products by combining high-pressure coal water slurry radiation waste boiler type gasification and low-pressure ammonia synthesis comprises the following steps:
1) steam generated by the boiler unit provides driving power for the air separation unit, and air is separated into at least oxygen and nitrogen by adopting a low-temperature rectification method;
2) the oxygen obtained by separation in the step 1 is used as a gasifying agent, and is subjected to gasification reaction with the coal water slurry prepared by the coal water slurry preparation unit at a high-pressure coal water slurry radiation waste boiler type gasification unit with a reaction pressure of 8.0-8.7 MPa, heat exchange is carried out, crude synthesis gas with a pressure of 7.8-8.5 MPa is discharged, and a high-pressure saturated steam with a pressure higher than 9.0MPa is obtained as a byproduct;
3) conveying the crude synthesis gas to a conversion unit, and discharging conversion gas with the pressure of 7.6-8.3 MPa, medium-pressure saturated steam with the pressure of 5.0-8.5 MPa and low-pressure saturated steam with the pressure of 0.5-2.5 MPa;
4) the converted gas is conveyed to a low-temperature methanol washing unit to at least remove hydrogen sulfide and carbon dioxide, purified gas with the pressure of 7.5-8.2 MPa is discharged,
5) removing at least carbon monoxide and methane from the purified gas by a liquid nitrogen washing unit to discharge hydrogen;
6) and (3) directly conveying the mixed gas of the nitrogen obtained by the separation in the step (1) and the hydrogen product obtained in the step (5) to a low-pressure ammonia synthesis unit, carrying out ammonia synthesis reaction (the reaction pressure is 7.2-8.0 MPa) under the action of ZA-5 type catalyst, and cooling the generated ammonia gas to obtain liquid ammonia.
Application example
The method of the invention is adopted to synthesize ammonia products, and industrial bypass tests are carried out in a low-pressure ammonia synthesis unit.
The experimental results are as follows:
table one: inlet gas component of industrial bypass experiment synthetic tower
| Synthesis gas | H2 | N2 | H2/N2 | Ar | CH4 | He | CO+CO2 | NH3 |
| Content% | 68～70 | 26～28 | 2.4～2.65 | 0.07 | 0.01 | 1.59 | ≤10×10-4 | 3.5～3.7 |
Table two: ZA-5 catalyst Activity
Outlet ammonia concentration was 8 hour average, as follows.
Conclusion of the bypass test: under the pressure of 7.0-7.5 MPa, the concentration of the outlet ammonia of the ZA-5 catalyst is 15.4-15.8%, and the net ammonia value is 11.7-13.2%, so that the requirement of industrial economy of synthetic ammonia on the net ammonia value (more than 8.4) can be met, and the method disclosed by the invention is feasible.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (8)
1. A method for preparing ammonia products by combining high-pressure coal water slurry radiation waste boiler type gasification with low-pressure ammonia synthesis is characterized by comprising the following steps:
1) superheated steam generated by the boiler unit provides driving power for the air separation unit, and air is separated into at least oxygen and nitrogen by adopting a low-temperature separation technology;
2) the oxygen is used as a gasifying agent and is subjected to gasification reaction with the coal water slurry prepared by the coal water slurry preparation unit in a high-pressure coal water slurry radiation waste boiler type gasification unit and heat exchange to obtain crude synthesis gas and by-product high-pressure steam;
3) the crude synthesis gas is conveyed to a conversion unit, carbon monoxide in the crude synthesis gas is converted into hydrogen to obtain conversion gas, and medium-pressure saturated steam and low-pressure saturated steam are produced as byproducts;
4) the converted gas is conveyed to a low-temperature methanol washing unit, and at least hydrogen sulfide and carbon dioxide in the converted gas are removed to obtain purified gas;
5) the purified gas is sent to a liquid nitrogen scrubbing unit to remove at least a small amount of carbon monoxide and methane from the purified gas to obtain CO and CO2A hydrogen product having a content of less than 10 PPm;
6) and (3) directly conveying the nitrogen obtained by the separation in the step (1) and the hydrogen product obtained in the step (5) to a low-pressure ammonia synthesis unit, carrying out ammonia synthesis reaction under the action of ZA-5 type catalyst, and cooling the generated ammonia gas to obtain liquid ammonia.
2. The method for preparing ammonia products by combining high-pressure coal water slurry radiation waste boiler type gasification and low-pressure ammonia synthesis according to claim 1, wherein in the step 2, the reaction pressure of a combustion chamber of a gasification furnace of the coal water slurry radiation waste boiler type gasification unit is 8.0-8.7 MPa.
3. The method for preparing ammonia products by combining high-pressure coal water slurry radiation waste pot type gasification with low-pressure ammonia synthesis according to claim 1, wherein the pressure of the obtained raw synthesis gas in the step 2 is 7.8-8.5 MPa.
4. The method for preparing ammonia products by combining high-pressure coal water slurry radiation waste boiler type gasification and low-pressure ammonia synthesis according to claim 1, wherein the pressure of the obtained conversion gas in the step 3 is 7.6-8.3 MPa.
5. The method for preparing ammonia products by combining high-pressure coal water slurry radiation waste boiler type gasification and low-pressure ammonia synthesis according to claim 1, wherein the pressure of the purified gas obtained in the step 4 is 7.5-8.2 MPa.
6. The method for preparing the ammonia product by combining high-pressure coal water slurry radiation waste boiler type gasification and low-pressure ammonia synthesis according to claim 1, wherein in the step 6, the feeding molar ratio of the hydrogen product to the nitrogen is 2.0-2.5, the reaction pressure is 7.2-8.0 MPa, and the highest reaction temperature is not more than 460 ℃.
7. The method for preparing ammonia products by combining high-pressure coal water slurry radiation waste boiler type gasification and low-pressure ammonia synthesis according to claim 1, wherein in the step 2, high-pressure steam obtained by the high-pressure coal water slurry radiation waste boiler type gasification unit is preheated and then is changed into superheated power steam which is used for providing driving power for the air separation unit.
8. The method for preparing ammonia products by combining high-pressure coal water slurry radiation waste boiler type gasification and low-pressure ammonia synthesis as claimed in claim 1, wherein in step 6, the purge gas discharged by the low-pressure ammonia synthesis unit is returned to the low-pressure ammonia synthesis tower after being pressurized.
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