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    • 专利摘要:
    "METHOD AND APPARATUS FOR DEHYDRATION AND DESULFURIZATION OF AND REMOVAL OF GAS DUST FROM THE FCC TAIL THROUGH AMMONIA-BASED PROCESS" The present invention relates to an apparatus and method for denitrating and desulphurizing and removing dust from an FCC tail gas by an ammonia-based process. The apparatus comprises a first stage waste heat recovery system, a denitration system, a dust removal and desulfurization system, a tail gas exhaust system and an ammonium sulphate post-processing system. The dust removal and desulfurization system comprises a separate dust removal tower and absorption tower. The upper and lower parts of the absorption tower are connected respectively to the tail gas exhaust system and to the ammonium sulphate post-processing system. The absorption tower comprises, in sequence, from the bottom upwards, an oxidation section, an absorption section and a fine particle control section. The method for denitration and desulfurization and dust removal from an FCC tail gas (...).
    公开号:BR102017013544B1
    申请号:R102017013544-6
    申请日:2017-06-22
    公开日:2020-11-10
    发明作者:Jing Luo；Jun Zhang；Yongying LUO；Qiang Tan；Xiangjun Xu
    申请人:Jiangnan Environmental Protection Group Inc.；
    IPC主号:
    专利说明:

    TECHNICAL FIELD
    [0001] The present invention relates to the field of environmental protection technologies and, in particular, to a method and system for denitrating and desulphurizing and removing dust from a residual FCC gas through an ammonia-based process . BACKGROUND
    [0002] SO2, NOx and dust are the main pollutants in the atmosphere and are a significant source of air pollution. With the increased load of total industrial pollution and limited environmental receptivity, emission standards need to be further refined to reduce the concentration of pollutants emitted. Fluidized Catalytic Cracking (FCC) residual gas is characterized by a large fine particle level (particles with a size of 0-10 pm are responsible for 50% or more) and high SO2 concentration (300-4500 mg / m3). In addition, the dust level fluctuates a lot, particularly when the catalyst loss occurs in a regenerator during the regular soot blowing process and in a state of accident of a high temperature economizer, the dust level is increased dramatically . In addition to silicon, aluminum and other metallic elements, the powder also contains nickel, vanadium and other heavy metal elements, thereby affecting the quality of by-products, and affecting the recovery of sulfur resource. All of these factors increased the difficulty in effectively managing the flue gas pollution that occurs during the catalyst regeneration of a catalytic cracking unit.
    [0003] Following stricter environmental protection standards and policies by power, steel and other industries have been intensively formulated in recent years, the Minister of Environmental Protection of the People's Republic of China issued the “Emission standard of pollutants for petroleum refining industry” (GB31570-2015) on April 16, 2015, which establishes stricter requirements on the emission of the main pollutants in FCC regenerative flue gas (FCC residual gas), where the specific emission limits for NOx, SO2 and matter in particle size are adjusted to 100 mg / m3, 50 mg / m3 and 30 mg / m3. In this way, desulfurization, desulfurization and dust removal of the FCC regenerative flue gas is a very difficult task, and it is imperative to develop a more efficient deep denitrification, desulfurization and dust removal process and technology with the recovery of sulfur resource, in order to meet the most stringent environmental protection requirements.
    [0004] At present, the removal of dust from and desulfurization of the FCC regenerative flue gas in China is mainly based on the use of wet wash technology; however, the investment, operation and maintenance costs are high and the system construction period is long. In addition, these technical methods also have problems such as high consumption of bleach, large volume of waste water and others. The existing popular sodium process is a disposable process; where the desulfurization and dust removal operations do not need to be separated; however, high salt waste water needs to be treated, secondary pollution is caused, and a large amount of catalyst enters the washing liquid under the condition of catalyst loss operation, which not only increases the treatment load of the solid. waste, and also causes the loss of the catalyst, thereby affecting the long-term stable operation of the system. In view of this, FCC regenerative combustion gas pollution treatment technologies have also been studied and developed in China in recent years. Chinese Patent Application No. CN 104941423A discloses a method and system for denitrating and desulphurizing and removing dust from an FCC regenerative flue gas through an ammonia-based process on September 30, 2015. The method includes the high temperature flue gas inlet steps containing the catalyst powder produced during the catalyst regeneration of a catalytic cracking unit in a waste heat recovery boiler I, where the flue gas temperature is reduced to 280- 430 ° C and the flue gas heat is used by the waste heat recovery boiler I to produce steam for the outlet; flue gas entry at 280-430 ° C in a denitration unit for denitration; after adequate reaction on the surface of the denitration catalyst in the denitration reactor, entry of the flue gas into a waste heat recovery boiler II through flue gas ventilation; removal of sulfur dioxide and nitrogen oxide in the flue gas through reaction with ammonia, with ammonium sulfate being produced as a by-product, and removal of the catalyst powder in the flue gas at the same time, to obtain a clean gas that is discharged to standard.
    [0005] In the method, an integrated desulfurization and dust removal technology using an ammonia-based process is employed. Although the process is simple, the obstacles during operation are less, the space occupied by the device is small and the investment and operation costs are saved, the applicant finds during the operation and long-term practice that where the same absorption liquid is used for dust removal and desulfurization, the absorption liquid containing ammonium sulphate is difficult to separate from the powder because the particle size of the catalyst powder is small. In order to ensure the quality of the ammonium sulphate product, the separation process needs to be strengthened, resulting in an increased investment and operating cost of the separation process. The method requires that the level of dust in the flue gas at the inlet is 30-800 mg / Nm3. Dust removal and desulfurization are carried out at the same time, and there is mutual interference, thereby affecting the long-term stable operation of the system. Especially when the level of dust in the flue gas at the inlet is as high as 5000 mg / Nm3 and the total amount exceeds 2 tons under an accident condition, the ingredients that enter the absorption liquid in circulation will affect the absorption liquid, and the desulfurization and dust removal efficiencies, and the absorption liquid cannot be effectively separated from the powder, thus affecting the quality of the ammonium sulphate product.
    [0006] There is an urgent need for technology for deep denitration, desulphurisation and dust removal of the recovery type to overcome the inconveniences existing in the existing technique. SUMMARY OF THE INVENTION
    [0007] In order to solve the technical problems in the prior art that through the existing process for denitrating and desulphurizing and removing dust from a residual FCC gas using an ammonia-based method, only raw flue gas having a level powder of 30-800 mg / Nm3 can be treated, causing a narrowed scope of applicability of the process; the quality of the ammonium sulphate by-product is difficult to ensure, and if the separation process is reinforced, the investment and operating cost will be increased; and dust removal and desulfurization are carried out at the same time, so that the system has difficulty operating stably for a long period of time, and a large amount of catalyst enters the washing liquid under a loss-of-operation condition. catalyst, causing the increased treatment load of the refuse solid and the catalyst refuse, the present invention provides a system and method for denitrating and desulphurizing and removing dust from a residual FCC gas through an ammonia-based process . The system for denitrating and desulphurizing and removing dust from a residual FCC gas through an ammonia-based process according to the present invention can operate stably for a long period of time. The ammonium sulphate by-product obtained from the method for denitrating and desulphurising and removing dust from a residual FCC gas through an ammonia-based process according to the present invention has high quality, high desulphurization rate, rate of high denitration and high dust removal rate and clean flue gas meets the requirements as specified by GB31570-2015 "Emission standard of pollutants for petroleum refining industry".
    [0008] In the present invention, the technical solutions that follow are employed to solve the above technical problems.
    [0009] A technical solution of the present invention is to provide a system for denitrating and desulfurizing and removing dust from a residual FCC gas through an ammonia-based process. The system includes a first stage waste heat recovery unit, a denitration unit, a dust removal and desulfurization unit, a residual gas exhaust unit and an ammonium sulphate post-processing unit. The denitration unit has a feed port for a denitration reducing agent provided therein. The dust removal and desulphurisation unit includes a dust removal tower and an separately arranged absorption tower. The upper and lower parts of the absorption tower are connected respectively to the waste gas exhaust unit and the ammonium sulphate post-processing unit. The dust removal tower is provided with at least 2 layers of washing liquid sprayers and at least one layer of mist separators is provided above the washing liquid sprayers in the dust removal tower. The absorption tower sequentially includes, from the bottom upwards, an oxidation section, an absorption section and a fine particle control section, where the absorption section is provided with at least 2 layers of sprayers in the absorption section, and the fine particle control section is provided with 1 to 4 layers of washing cyclically with diluted ammonium sulfate solution.
    [0010] In the present invention, the first stage waste heat recovery unit, the denitration unit, the dust removal tower and the absorption tower are connected in a relationship that is conventional in the art; and, preferably, the first stage waste heat recovery unit, the denitration unit, the dust removal tower and the absorption tower are connected in sequence.
    [0011] Preferably, the system for denitrating and desulphurizing and removing dust from a residual FCC gas through an ammonia-based process according to the present invention further includes a second stage waste heat recovery unit, where the first stage waste heat recovery unit, the denitration unit, the second stage waste heat recovery unit, the dust removal tower and the absorption tower are connected in sequence.
    [0012] In the present invention, the denitration unit is a denitration unit for a residual FCC gas through an ammonia-based process conventionally used in the art. Preferably, the denitration unit is a selective catalytic reduction reactor (SCR), where a rectifier is provided in an upper part of the SCR reactor and an ammonia injection grid is provided in an inlet for the residual FCC gas of the SCR reactor. .
    [0013] The functions of the oxidation section, the absorption section and the fine particle control section in the absorption tower are similar to those described in Chinese Patent Applications Nos. CN103301705B entitled "Apparatus and method for controlling fine particles in flue gas for desulfurization" and CN104524948B entitled "Ultra-low discharge method for integrated ultrasonic desulfurization and dust removal" deposited by the present applicants. The present invention is advantageous in that the removal of dust through washing with water and desulfurization through an ammonia-based process are carried out in 2 separate towers. 80% or more of dust is removed in the dust removal tower, so that product quality and the final dust emission index are ensured. Correspondingly, no cooling and washing sections need to be provided in the absorption tower.
    [0014] In the present invention, 2 to 5 layers of washing liquid sprayers are preferably provided in the dust removal tower, where the liquid to gas ratio between each layer of the washing liquid sprayers is not less than 1, 1 L / m3, the spray coverage rate is not less than 120% and the total spray coverage rate of the dust removal tower is not less than 200%. The dust removal tower preferably comprises 1 to 5 layers of mist separators.
    [0015] The mist separator of the dust removal tower is a mist separator conventionally used in the art and preferably one or more of a mist separator with deflector, a mist separator with a ceiling and a mesh mist separator.
    [0016] In the present invention, the lower part of the dust removal tower is preferably connected still to a washing circulation pump, which is connected to a filtering unit. The filter unit is connected to the top of the dust removal tower and the absorption tower respectively. An inlet for process water to the dust removal tower is provided to an upper portion of the dust removal tower.
    [0017] Fresh process water or evaporated condensed water is added to the dust removal tower via the process water inlet to the dust removal tower and a circulating washing liquid enters. A portion of the circulating washing liquid passes through the filter unit and enters the absorption tower.
    [0018] In the present invention, the absorption spray liquid is collected in the oxidation section and oxidized with air. Most of the slurry is recycled and a portion of the slurry enters the ammonium sulphate post-processing unit, where an ammonium sulphate product is obtained. The recycling slurry and the slurry entering the ammonium sulphate post-processing unit for evaporation and recrystallization are removed from different positions in the oxidation section. Preferably, the oxidation section is provided with 3 to 8 layers of gas-water dispersion enhancers.
    [0019] In the present invention, the absorption tower preferably comprises 2 to 4 layers of sprayers in the absorption section, where the liquid to gas ratio between each layer of the sprayers in the absorption section is not less than 1.1 L / m3, the spray coverage rate is not less than 120% and the total spray coverage rate of the absorption section is not less than 300%.
    [0020] In the present invention, more than 1 layer of mist separators is preferably provided above the sprayers in the absorption section; and still preferably, the absorption section comprises 1 to 5 layers of mist separators.
    [0021] The absorption section mist separator is a mist separator conventionally used in the art and preferably one or more of a deflector mist separator, a ceiling type mist separator and a mesh mist separator.
    [0022] In the present invention, the cyclic wash layer with diluted ammonium sulfate solution is conventional in the art. Preferably, the cyclic wash layer with diluted ammonium sulfate solution is provided with more than 1 layer of sprayers in the wash layer, and more than 1 layer of mist separators is provided above the sprayers in the wash layer, where the ratio of liquid to gas between each layer of the sprayers in the wash layer is not less than 1.1 L / m3, the spray coverage rate is not less than 120% and the total spray coverage rate of the control section of fine particle is not less than 300%. Most preferably, the wash layer comprises 1 to 4 layers of sprayers and 1 to 5 layers of mist separators.
    [0023] The wash layer mist separator is a mist separator conventionally used in the art and preferably one or more of a mist separator with deflector, a roof type mist separator and a mesh mist separator.
    [0024] In the present invention, the lower part of the absorption tower is connected with at least one absorption circulation pump and the absorption section of the absorption tower has an inlet for absorption spray liquid provided therein. Preferably, 2 absorption circulation pumps are present, where several branches coming from one of the absorption circulation pumps are connected respectively to the intake for the absorption spray liquid of the absorption tower and the ammonium sulphate post-processing unit ; and the other absorption circulation pump is directly connected to the intake for the absorption spray liquid of the absorption tower. An inlet for process water for the absorption tower is provided in an upper portion of the absorption tower and an entrance for an absorbent containing ammonia and an entrance for air as an oxidizer is provided in a lower portion of the absorption tower.
    [0025] Fresh process water or evaporated condensed water is added to the absorption tower through the process water inlet to the absorption tower.
    [0026] After sulfur dioxide is absorbed in the absorption section, the residual FCC gas enters the fine particle control section and is cyclically washed with diluted ammonium sulphate solution to absorb the fine particles (including fine ingrained powder particles) in residual FCC gas, escaped ammonia and aerosol), where the size of the fine particles is <1 pm.
    [0027] In the present invention, the residual gas exhaust unit is conventional in the art and disposed lateral to or above the desulfurization unit. The waste gas exhaust unit is preferably a waste gas exhaust flue when disposed on top of the desulfurization unit.
    [0028] In the present invention, the ammonium sulfate post-processing unit is conventional in the art. Preferably, the ammonium sulphate post-processing unit includes an evaporation and crystallization device, a cyclone, a centrifuge, a dryer and a packaging machine connected in sequence, where the evaporation and crystallization device is connected to the absorption tower. .
    [0029] In the present invention, the external part, the internal components and tubes of the dust removal tower, the absorption tower and the evaporation and crystallization device are all made with a corrosion resistant material and preferably with a steel material Grade 022Cr17Ni12Mo2 stainless steel, Grade 00Cr22Ni5Mo3N double phase steel material, Grade 00Cr25Ni6Mo2N dual phase steel material, a titanium based material or Q235B steel coated with epoxy glass flakes.
    [0030] The connection relationship in the system above will be described below.
    [0031] The first stage waste heat recovery unit and the denitration unit are connected in a relationship that is conventional in the art. In general, an output from the first stage waste heat recovery boiler is connected to a gas inlet of the denitration unit; and an outlet from the denitration unit is connected to the second stage waste heat recovery unit.
    [0032] Another technical solution of the present invention is to provide a method for denitrating and desulphurizing and removing dust from a residual FCC gas through an ammonia-based process, using the system for denitrating and desulphurizing and removing dust. residual FCC gas through an ammonia-based process. The method comprises the steps of: (1) entry of the FCC gas sequentially into the first stage waste heat recovery unit and the denitration unit for cooling and denitration, respectively, where the temperature of the residual gas is reduced to 250- 350 ° C; (2) after treatment in the denitration unit, entry of residual FCC gas discharged into the dust removal and desulphurisation unit after passing through a second stage waste heat recovery unit, for removing dust in the dust removal tower and desulfurization in the absorption tower, respectively; and (3) discharge of the clean residual gas after desulfurization through the waste gas exhaust unit and collection of the ammonium sulphate by-product in the ammonium sulphate post-processing unit.
    [0033] In the present invention, the temperature of the residual FCC gas entering the first stage waste heat recovery unit is from 580 to 950 ° C, the NOX concentration is 100 to 1200 mg / Nm3, the SO2 concentration is 200 to 30000 mg / Nm3 and the total powder level is 50 to 10,000 mg / Nm3. Preferably the temperature of the residual FCC gas entering the first stage waste heat recovery unit is from 600 to 670 ° C, the NOX concentration is 250 to 800 mg / Nm3, the SO2 concentration is 500 at 5000 mg / Nm3 and the total powder level is 100 to 300 mg / Nm3.
    [0034] In the present invention, the denitration in Step (1) is performed following a conventional denitration process in the art and preferably following a selective catalytic reduction (SCR) process or a selective non-catalytic reduction process (SNCR). The reducing agent used during denitration is conventional in the art and preferably ammonia and / or urea.
    [0035] In the present invention, the temperature of the residual FCC gas after being further cooled in the second stage waste heat recovery unit in Step (1) is preferably from 140 to 220 ° C.
    [0036] When the second stage waste heat recovery unit is employed for additional cooling of the residual FCC gas, the residual FCC gas discharged after treatment in the second stage waste heat recovery unit is fed into the unit dust removal and desulfurization, where the residual FCC gas is cooled more by the second stage waste heat recovery unit in such a way conventional in the art than a low pressure steam of 0.3 to 0.8 MPa and a Preheated soft water is preferably produced as by-products.
    [0037] In the present invention, desulfurization in Step (2) is carried out following a conventional desulfurization process in the art. During the desulfurization process in Step (2), a lower absorption liquid is collected at the bottom of the absorption tower, part of which is fed to the ammonium sulphate post-processing unit and the other part of which is oxidized with an oxygen-containing gas, replaced with an ammonia-containing absorbent, and then recycled to the absorption section of the absorption tower.
    [0038] Preferably, the oxygen-containing gas is preferably air.
    [0039] Preferably, the ammonia-containing absorbent is preferably 10-25% by weight aqueous ammonia and / or liquid ammonia.
    [0040] Preferably, the lower absorption liquid recycled to the absorption section makes up 75-98% by weight of the total lower absorption liquid.
    [0041] In the clean flue gas obtained through the method for denitration and desulfurization and removal of dust from a residual FCC gas through an ammonia-based process according to the present invention, the NOX concentration is <100 mg / Nm3, the SO2 concentration is <50 mg / Nm3, the total dust level is <20 mg / Nm3 and the dust removal efficiency is not less than 80%.
    [0042] The quality of the ammonium sulfate by-product obtained from the method for denitration and desulphurisation and removal of dust from a residual FCC gas through an ammonia-based process according to the present invention meets the requirements as specified by GB535-1995.
    [0043] The preferred conditions described above can be arbitrarily combined to obtain preferred examples of the present invention, based on common knowledge in the art.
    [0044] The reagents and particle materials used in the present invention are commercially available.
    [0045] The present invention has the following positive effects. The process of the present invention has no waste water discharge and no secondary pollution, allows synergistic control of various pollutants and recovery of sulfur dioxide through resource recovery to obtain the finished product ammonium sulfate and can reduce the cost of investment and operation and operate stably for a long period of time. BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWINGS
    [0046] Fig. 1 is a flow chart of the process of Example 1.
    [0047] Fig. 2 is a schematic structure view of a system for denitrating and desulphurizing and removing dust from a residual FCC gas through an ammonia-based process provided in Example 1.
    [0048] List of numerals: In figure 1: 6: ammonium sulphate post-processing unit; 7: ammonia; 8: residual FCC gas; 9: ammonium sulfate; 10: clean residual gas; 123: waste denitration and heat recovery unit; 44: dust removal unit; 45: desulfurization unit; In Figure 2: 1: first stage waste heat recovery unit; 2: denitration unit; 3: second stage waste heat recovery unit; 4: dust removal and desulfurization unit; 5: residual gas exhaust unit; 6: ammonium sulphate post-processing unit; 11: input for residual FCC gas; 21: feeding port for denitration reducing agent; 41: dust removal tower; 42: absorption tower; 421: inlet for absorbent containing ammonia; 422: entry to air as an oxidizer; 61: evaporation and crystallization device; 62: cyclone; 63: centrifuge; 64: dryer; 65: packaging machine. DETAILED DESCRIPTION
    [0049] Hereinafter, the present invention is illustrated further by way of examples; however, the present invention is not limited to them. The experimental methods in the examples that follow where any specific conditions are given are implemented according to conventional methods and conditions or selected according to the product specification.
    [0050] In GB535-1995, the parameters required for ammonium sulphate of the first degree are: N content> 21%, water content <0.3% and free acid content <0.05%.
    [0051] In Example 1 below, the process flow is as follows. A residual gas of FCC 8 enters a denitration and waste water recovery unit 123 for the purpose of denitration under the action of ammonia 7. The residual FCC gas after denitration enters a dust removal unit 44 and then enters in a desulphurization unit 45 for additional desulphurization under the action of ammonia 7. The clean residual gas 10 after desulphurisation is charged through a residual gas processing unit and the remaining circulating liquid enters the ammonium sulphate post-processing unit 6, where ammonium sulfate 9 is obtained. The specific process is shown in Fig. 1. Example 1
    [0052] This example provides a system for denitrating and desulphurizing and removing dust from a residual FCC gas through an ammonia-based process, which has a processing capacity of 100,000 ton / year. The system includes a first stage waste heat recovery unit 1, a denitration unit 2, a second stage waste heat recovery unit 3, a dust removal and desulphurisation unit 4, a dust extraction unit residual gas 5 and an ammonium sulphate post-processing unit 6. The first stage waste heat recovery unit 1 has an inlet 11 of the FCC cause gas provided thereto. The denitration unit 2 is connected to the first stage 1 waste heat recovery unit and has a feed port 21 of a denitration reducing agent in it. The second stage 3 waste heat recovery unit is connected to the denitration unit. The dust removal and desulfurization unit 4 includes a dust removal unit and a desulfurization unit arranged separately. In this example, the dust removal unit is a dust removal tower 41 connected to the second stage 3 waste heat recovery unit; and the desulfurization unit is an absorption tower 42 connected to the dust removal tower 41 and also to the residual gas exhaust unit 5 and to the ammonium sulphate post-processing unit 6, respectively. The absorption tower 42 has an inlet 421 for an ammonia-containing absorber and an inlet 422 for air as an oxidizer provided therein, specifically as shown in Fig. 2.
    [0053] In this example, the dust removal tower is provided with 3 layers of washing liquid spray, where the liquid to gas ratio between each layer of the washing liquid sprayers is 1.5 L / m3, the rate spray coverage of each single layer is 140% and the total spray coverage rate of the dust removal tower is not less than 400%. The dust removal tower is provided with 2 layers of mist separators in an upper part of the dust removal tower, which are deflector and ceiling type mist separators. The dust removal efficiency of the dust removal tower is not less than 80%. The washing liquid containing solid obtained in the dust removal tower is fed to the filter unit for removing solid and the washing liquid removed from the solid is recycled for washing the residual FCC gas.
    [0054] In this example, an oxidation tank is provided at the bottom of absorption tower 42, and 3 layers of absorption liquid sprayers are provided in an absorption section above the inlet for the flue gas, where the ratio of liquid to gas between each layer of the washing liquid sprayers is 1.25 L / m3, the spray coverage rate for each single layer is 130% and the total spray coverage rate for the dust removal tower is 320% . The absorption liquids of different oxidation rates are taken from 2 different positions of the oxidation tank at the bottom of the absorption tower, one of which is recycled for absorption by an absorption circulation pump and the other of which is fed to a evaporation and crystallization unit. A fine particle control section is provided above the absorption section and the fine particle control section includes 2 layers of mist separators provided above a spray layer in a wash layer and the mist separators in the wash layer they are mist separators of the ceiling and mesh type.
    [0055] In this example, the ammonium sulphate post-processing unit 6 includes an evaporation and crystallization device 61, a cyclone 62, a centrifuge 63, a dryer 64 and a packaging machine 65 connected in sequence.
    [0056] In this example, the external part, the internal components and the tubes of the dust removal tower, the absorption tower and the evaporation and crystallization device are all made with a grade 022Cr17Ni12Mo2 stainless steel material.
    [0057] This example further provides a method for denitrating and desulfurizing and removing dust from a residual FCC gas using an ammonia-based process using the system for denitrating and desulfurizing and removing dust from a residual FCC gas. through an ammonia-based process. The method comprises the steps of: (1) FCC residual gas inlet, where the flow rate is 262000 Nm3 / h, the FCC residual gas temperature is 600-650 ° C, the dust level in the flue gas is 200 mg / Nm3 m a normal case, the SO2 concentration is 3550 mg / Nm3, the NOX concentration is 350 mg / Nm3, the powder level is 7500 mg / Nm3 under the condition of operation and loss of catalyst, the catalyst loss duration is 2.5 h and catalyst loss is 4.91 t, in the first stage waste heat recovery unit where the FCC waste gas temperature is reduced to 335 ° C and the waste gas heat it is used by the first stage waste heat recovery unit to produce 4 MPa steam at a rate of 11.6 t / h for output; (2) flue gas inlet at 335 ° C in the denitration and denitration unit with 5-15% aqueous ammonia, where after adequate reaction on the denitration catalyst surface in the denitration reactor, the nitrogen oxide content is decreased to 35 mg / Nm3 and the denitration rate is 90%. (3) after treatment in the denitration unit, flue gas enters the second stage waste heat recovery unit through flue gas ventilation, where 0.6 MPa steam is produced at 3.3 t / h as a by-product and the flue gas temperature is reduced to 166 ° C in the second stage waste heat recovery unit; (4) after treatment in the second stage waste heat recovery unit, entry of residual FCC gas discharged into the dust removal tower for dust removal and the absorption tower for desulfurization, where the washing liquid containing solid obtained in the dust removal tower is fed to a filtering unit for removing solids and the washing liquid removed from the solid is recycled to wash the residual FCC gas; and the residual FCC gas entering the absorption tower is desulfurized with 5-15% aqueous ammonia; and (5) after desulphurisation, discharge of the flue gas through the residual gas exhaust unit, where the NOx content is 35 mg / Nm3, the SO2 content is 38 mg / Nm3, the dust level is 11 , 5 mg / Nm3 in a normal case and is 21 mg / Nm3 under the condition and catalyst loss operation; the 40% ammonium sulphate solution produced as a by-product at about 4.7 t / h is evaporated and recrystallized, vortexed, centrifuged, dried and packaged, to obtain a 1.89 t / ammonium sulphate finished product h, whose quality (nitrogen content: 21.05%, water content: 0.2% and free acid content: 0.03%) meets the requirements of first grade ammonium sulphate as specified by GB535-1995 .
    [0058] The list of methods and main instruments for detecting various indexes in this example is shown in Table 1. The parameters of the main raw materials and the product are shown in Table 2. Table 1: list of methods and main instruments for detection of various indexes
    (Table 1 - Continued)
    Table 2: parameters of main raw materials and product
    (Table 2 - Continued)

    [0059] The desulfurization efficiency in this example is 98.9% and the denitration efficiency is 90%. Comparative Example 1
    [0060] CN104941423A is obtained as a comparative example, where the flue gas of 100.0000 ton / year produced during the catalyst regeneration of a catalytic cracking unit is treated, where the flue gas flow rate is 135000 Nm3 / h , the temperature is 950 ° C, the moisture content is 12%, the nitrogen oxide concentration is 360 mg / Nm3, the sulfur dioxide concentration is 2300 mg / Nm3, the powder level is 150 mg / Nm3 and the desulfurizing agent is 99.6% liquid ammonia. In a normal case, the denitration efficiency is 88.9%, the desulfurization efficiency is 98.5%, the NOX concentration in the clean flue gas is 38 mg / Nm3, the concentration and SO2 is 32 mg / Nm3, The powder level is less than 15 mg / Nm3 and the nitrogen content in the ammonium sulfate by-product is 20.8%.
    [0061] However, the operating condition of catalyst loss is not taken into account. In this case, if the flue gas is treated with the system according to Chinese Patent No. CN 104941423A, the following effects are finally achieved.
    [0062] A large amount of powder enters the absorption liquid, so that the insoluble solid content in the absorption liquid increases to 3% or more. This causes the ammonium sulfate product to fail to be recrystallized and discharged. Even if the ammonium sulphate product could be discharged, the N content in the product would be reduced to 18% or below and thus the product cannot be marketed. In addition, the absorption circulation pump is clogged and worn, and the system must be turned off to clean the solids accumulated in the absorption tower.
    [0063] The effects of the present invention are as follows. The denitration efficiency is> 90%, the desulphurization efficiency is 98.9%, the NOx concentration in the clean flue gas is 35 mg / Nm3, the SO2 concentration is 38 mg / Nm3, the powder level is 11 , 5 mg / Nm3 and the nitrogen content in the ammonium sulfate by-product is 21.06%. The system of the present invention can operate normally under the catalyst loss operation condition and is obviously advantageous over that of the Comparative Example, as indicated by a powder level at the outlet of 21 mg / Nm3.
    权利要求:
    Claims (10)
    [0001]
    1. System for denitration, and desulphurization and removal of dust from a residual gas from Fluidized Catalytic Cracking (FCC) (8) through an ammonia-based process, characterized by the fact that it comprises a waste heat recovery unit first stage (1), a denitration unit (2), a dust removal and desulfurization unit (4), a residual gas exhaust unit (5), and an ammonium sulphate post-processing unit ( 6), in which the dust removal and the desulfurization unit (4) comprise a separate dust removal tower and absorption tower, in which the upper and lower parts of the absorption tower are connected to the unit respectively. exhaust gas exhaust (5) and the ammonium sulphate post-processing unit (6); the dust removal tower is provided with at least 2 layers of washing liquid sprayers, and at least one layer of mist separators is provided above the washing liquid sprayers in the dust removal tower; and the absorption tower sequentially comprises, from the bottom upwards, an oxidation section, an absorption section and a fine particle control section, where the absorption section is provided with at least 2 layers of sprayers in the absorption section , and the fine particle control section is provided with 1 to 4 layers of washing in a cyclic manner with diluted ammonium sulfate solution, in which the first stage waste heat recovery unit (1), the denitration unit (2), the dust removal tower and the absorption tower are connected in sequence.
    [0002]
    2. System for denitrating and desulphurizing and removing dust from a residual FCC gas (8) using an ammonia-based process, according to claim 1, characterized by the fact that it also comprises a heat recovery unit second stage refuse unit (3), where the first stage refuse heat recovery unit (1), the denitration unit (2), the second stage refuse heat recovery unit (3), the dust removal tower and absorption tower are connected in sequence.
    [0003]
    3. System for denitrating and desulfurizing and removing dust from a residual FCC gas (8) using an ammonia-based process, according to claim 1, characterized by the fact that the denitration unit (2) is a selective catalytic reduction reactor, in which a rectifier is provided in an upper part of the selective catalytic reduction reactor, and an ammonia injection grid is provided in an inlet for the residual FCC gas (8) of the catalytic reduction reactor selective.
    [0004]
    4. System for denitrating and desulphurizing and removing dust from a residual FCC gas (8) using an ammonia-based process, according to claim 3, characterized by the fact that the residual gas exhaust unit ( 5) is a waste gas exhaust flue.
    [0005]
    5. System for denitrating and desulphurizing and removing dust from a residual FCC gas (8) using an ammonia-based process according to claim 1, characterized by the fact that 2 to 5 layers of liquid sprayers washers are provided in the dust removal tower, in which the liquid to gas ratio between each layer of the wash liquid sprayers is greater than or equal to 1.1 L / m3, the spray coverage rate is greater than or equal to at 120% and the total spray coverage rate of the dust removal tower is greater than or equal to 200%; and the dust removal tower comprising 1 to 5 layers of mist separators; and / or the mist separator of the dust removal tower is one or more of a deflector mist separator, a cover type mist separator and a mesh type mist separator; and / or the oxidation section is provided with 3 to 8 layers of gas-liquid dispersion enhancers; and / or the absorption section comprises 2 to 4 layers of sprayers, where the liquid to gas ratio between each layer of sprayers in the absorption section is greater than or equal to 1.1 L / m3, the spray coverage rate is greater than or equal to 120% and the total spray coverage rate of the absorption section is greater than or equal to 300%; and / or the wash layer cyclically with diluted ammonium sulphate solution is provided with more than 1 layer of sprayers in the wash layer, and more than 1 layer of mist separators are provided above the sprayers in the wash layer, where the liquid-to-gas ratio between each spray layer in the wash layer is greater than or equal to 1.1 L / m3, the spray coverage rate is greater than or equal to 120% and the total spray coverage rate the fine particle control section is greater than or equal to 300%; and, preferably, the wash layer comprises 1 to 4 layers of sprayers and 1 to 5 layers of mist separators.
    [0006]
    6. System for denitrating and desulphurizing and removing dust from a residual FCC gas (8) using an ammonia-based process, according to claim 1, characterized by the fact that the sulphate post-processing unit Ammonium (6) comprises an evaporation and crystallization device, a cyclone, a centrifuge, a dryer and a packaging machine connected in sequence, in which the evaporation and crystallization device is connected to the absorption tower.
    [0007]
    7. Method for denitrating and desulphurizing and removing dust from a residual FCC gas (8) using an ammonia-based process, using the system for denitrating and desulphurising and removing dust from a residual FCC gas (8) ) through an ammonia-based process, as defined in any one of claims 1 to 6, characterized by the fact that it comprises the steps of: (1) inlet of the residual FCC gas (8) sequentially into the heat recovery unit first stage refuse (1) and in the denitration unit (2) for cooling and denitration, respectively, where the temperature of the residual gas is reduced to 250-350 ° C, and the temperature of the residual gas of FCC (8) entering the first stage waste heat recovery unit is 580 to 950 ° C, and the total dust level is 50 to 10,000 mg / Nm3; (2) after treatment in the denitration unit (2), discharge of residual FCC gas (8) from the discharge into the dust removal and desulfurization unit (4), for removing dust in the dust removal tower and desulfurization in the tower absorption, respectively; and preferably after treatment in the denitration unit (2), still heat recovery from the residual FCC gas (8) discharged into the second stage waste heat recovery unit (3), and then inlet of the residual gas FCC (8) discharged to the dust removal and desulfurization unit (4); and (3) discharge of the clean residual gas after desulfurization through the waste gas exhaust unit (5) and collection of the ammonium sulfate by-product in the ammonium sulfate post-processing system (6).
    [0008]
    8. Method for denitrating and desulphurizing and removing dust from a residual FCC gas (8) using an ammonia-based process according to claim 7, characterized by the fact that the temperature of the residual FCC gas ( 8) entering the first stage waste heat recovery unit (1) is from 580 to 950 ° C, the NOX concentration is 100 to 1200 mg / Nm3, the SO2 concentration is 200 to 30000 mg / Nm3 and the total powder level is 50 to 10,000 mg / Nm3; and preferably the temperature of the residual FCC gas (8) entering the first stage waste heat recovery unit (1) is from 600 to 670 ° C, the NOx concentration is 250 to 800 mg / Nm3 , the SO2 concentration is 500 to 5000 mg / Nm3 and the total powder level is 100 to 300 mg / Nm3.
    [0009]
    9. Method for denitrating and desulphurizing and removing dust from a residual FCC gas (8) using an ammonia-based process according to claim 7, characterized by the fact that the temperature of the residual FCC gas ( 8) after being cooled further in the second stage waste heat recovery unit (3) in Step (2) it is from 140 to 220 ° C; and when the second stage waste heat recovery unit (3) is employed for additional cooling of the residual FCC gas (8), the residual FCC gas (8) discharged after 0 treatment in the waste heat recovery unit second stage (3) is fed to the dust removal and desulfurization unit (4), in which the residual FCC gas (8) is further cooled by the second second stage waste heat recovery unit (3) in such a way so that the low pressure value of 0.3 to 0.8 MPa and a preheated soft water are produced as by-products.
    [0010]
    10. Method for denitrating and desulfurizing and removing dust from a residual FCC gas (8) using an ammonia-based process according to claim 7, characterized by the fact that during the desulfurization process in Step ( 2), a lower absorption liquid is collected at the bottom of the absorption tower, part of which is fed to the ammonium sulphate post-processing unit (6), and the other part of which is oxidized with a gas containing oxygen, supplemented with an absorbent containing ammonia, and then recycled to the absorption section of the absorption tower, where the oxygen-containing gas is preferably air; the ammonia-containing absorbent is preferably 10-25% by weight aqueous ammonia and / or liquid ammonia; and the lower absorption liquid recycled to the absorption section is preferably responsible for 75-98% by weight of the total lower absorption liquid.
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    同族专利:
    公开号 | 公开日
    US10092877B1|2018-10-09|
    MX2017008446A|2019-02-08|
    CN107213785A|2017-09-29|
    US20190282957A1|2019-09-19|
    CA2971738C|2018-06-26|
    EP3406320A1|2018-11-28|
    JP6397967B2|2018-09-26|
    US20180339266A1|2018-11-29|
    JP2018009781A|2018-01-18|
    CA2971738A1|2017-08-29|
    EP3406320B1|2020-08-12|
    CL2017001698A1|2018-02-16|
    WO2018214990A1|2018-11-29|
    US20190054419A1|2019-02-21|
    CN107213785B|2020-08-07|
    KR102022305B1|2019-09-18|
    KR20180129588A|2018-12-05|
    US10343110B2|2019-07-09|
    US10213739B2|2019-02-26|
    US10471383B2|2019-11-12|
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    法律状态:
    2017-10-03| B03B| Publication of an application: publication anticipated [chapter 3.2 patent gazette]|
    2018-01-30| B27A| Filing of a green patent (patente verde)|
    2018-03-13| B27B| Request for a green patent granted|
    2018-07-10| B07A| Technical examination (opinion): publication of technical examination (opinion) [chapter 7.1 patent gazette]|
    2018-09-04| B25A| Requested transfer of rights approved|Owner name: JIANGNAN ENVIRONMENTAL PROTECTION GROUP INC. (KY) |
    2019-03-12| B09B| Patent application refused [chapter 9.2 patent gazette]|
    2019-07-02| B12B| Appeal: appeal against refusal|
    2020-11-10| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 22/06/2017, OBSERVADAS AS CONDICOES LEGAIS. |
    优先权:
    申请号 | 申请日 | 专利标题
    CN201710379458.6A|CN107213785B|2017-05-25|2017-05-25|Method and device for denitration, desulfurization and dust removal of FCCtail gas by ammonia process|
    CN201710379458.6|2017-05-25|
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