An efficient and safe EG catalyst cleaning method and device
By adopting a cleaning method including a wet ball mill, a washing kettle and other devices in the preparation process of the EG catalyst industry, the problem of difficulty in cleaning semi-finished products during the preparation process of the EG catalyst industry is solved, cleaning efficiency and safety are improved, and the performance and production efficiency of the catalyst are enhanced.
Patent Information
- Application Number
- CN202411814998.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-11
- Publication Date
- 2025-04-04
AI Technical Summary
During the preparation of EG catalyst industry, semi-finished products have problems such as difficulty in beating filter cakes, long washing time, and difficult filter cake discharge during the conventional cleaning process, which affects the performance and production efficiency of the catalyst. At the same time, washing with hot water will cause ammonia to overflow, which poses safety hazards.
The device including a wet ball mill, a washing kettle, a hot water tank, a spray tower, a spray centrifugal pump, a gas-liquid separator, a vacuum pump, an ammonia water collection tank, a circulation centrifugal pump, a conveyor belt and a drying chamber is used to clean the EG catalyst through the steps of grinding, filtration, washing, bubbling and exhaust gas collection.
It improves the cleaning efficiency of EG catalysts, shortens washing time, reduces ammonia spillage, enhances safety, and improves the performance and production efficiency of the catalyst.
Smart Images
Figure CN119746948A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of EG catalyst cleaning, and in particular to an efficient and safe EG catalyst cleaning method and device. Background Art
[0002] The common method of EG catalyst is ammonia evaporation, which has the following specific steps: dissolving copper ingots with nitric acid to a certain concentration, then using ammonia water and urea with a certain concentration to react copper with ammonia, then adding a prepared silica gel mixture to evaporate ammonia, and filtering the filter cake after the ammonia evaporation reaction, washing, drying, grinding, granulating, drying, and baking. The catalyst obtained by this method has excellent activity and thermal stability.
[0003] The defect is that in the routine cleaning process of the semi-finished products in the industrial preparation process of EG catalyst, problems such as difficulty in filter cake slurrying, long washing time, and difficulty in filter cake discharge often occur, which affect the performance and production efficiency of the catalyst. Although professionals use hot water washing for optimization, the washing efficiency cannot be greatly improved. In addition, a large amount of ammonia overflows under hot water washing, which will cause safety hazards, not only endangering the breathing of on-site workers but also polluting the environment. Summary of the invention
[0004] The purpose of the present invention is to solve the above-mentioned problems and to propose an efficient and safe EG catalyst cleaning method and device.
[0005] In order to achieve the above object, the present invention adopts the following technical scheme: comprising a wet ball mill, a washing kettle, a hot water tank, a spray tower, a spray centrifugal pump, a gas-liquid separator, a vacuum pump, an ammonia water collection tank, a circulating centrifugal pump, a conveyor belt and a drying box;
[0006] The wet ball mill device includes a material connected to the ball mill, the lower end of the ball mill discharge port is connected to the lower end of the hot water tank pipe and flows into the washing kettle, wherein the ball mill is composed of two grinding balls connected to each other, and the lower end of the ball mill is a stainless steel filter. When the liquid particle size reaches the standard after grinding, it flows out through the filter and flows into the washing kettle along the pipeline, wherein the size of the stainless steel filter is 1-10um. The processing capacity of the ball mill is 50-300kg / min; the temperature of the hot water tank is 0-100℃;
[0007] The outer wall of the washing kettle is insulated by a steam jacket, the steam temperature in the jacket is 0-200°C, and it is heated by an annular steam pipe, and a temperature controller is installed inside, wherein the constant temperature required for the washing process is 30-80°C, a feed port with a valve is arranged at the upper end of the outer side of the washing kettle, a pipe port is arranged for the material filtered from the filter screen after grinding and mixed with hot water, a gas phase pipe is connected to the upper part of the right outer end of the washing kettle, a circular suction filter disc is arranged inside the washing kettle, the suction filter disc is made of thickened stainless steel, the orifice plate disc is funnel-shaped, a plurality of suction filter discs are arranged, a filter cloth is laid on the suction filter disc, an axial tube is arranged at the center of the suction filter disc, the axial tube is connected to each suction filter disc from top to bottom, and the axial tube is connected to a high-speed stirrer, a circulating centrifugal pump used in conjunction with the washing kettle is installed on one side of the washing kettle, an observation hole is arranged in the middle of the washing kettle, a nitrogen inlet valve is arranged at the lower left end of the washing kettle, a pneumatic pump is connected to the lower end of the washing kettle, and a drain valve and a solid discharge port are arranged at the lowest end of the washing kettle.
[0008] Hot water tank-wet grinder device
[0009] The material is connected to the ball mill feeder, and the lower end of the ball mill outlet is connected to the lower end of the hot water tank pipe and flows into the washing kettle. The ball mill has two grinding balls connected to each other for grinding. The lower end of the ball mill is a stainless steel filter. When the liquid particle size reaches the standard after grinding, it flows out through the filter and flows into the washing kettle along the pipeline. The size of the stainless steel filter is 1-10um. The processing capacity of the ball mill is 50-300kg / min; the temperature of the hot water tank is 0-100℃;
[0010] ②Composition of two washing kettles
[0011] A. The outer wall of the washing kettle is insulated with a steam jacket. The steam temperature in the jacket is 0-200℃, and it is heated by an annular steam pipe with a built-in temperature controller. The constant temperature required for the washing process is 30-80℃.
[0012] B. The upper outer side of the washing kettle: one of the feed ports has a valve, and the material filtered by the filter is mixed with hot water and then flows out of the pipe; the upper right outer end is connected to a gas phase pipe for discharge.
[0013] C. Working principle of the internal circular filter plate of the washing kettle: It is composed of multiple thickened stainless steel perforated discs, shaped like a Büchner funnel without a flat edge, and a filter cloth is laid on the top of the perforated plate. The center of the filter plate is connected by a central axis pipe from the first filter plate to the bottom layer. The central axis pipe is controlled by a high-speed agitator. The material flowing into the washing kettle is filtered on the mesh plate, and the permeated water is collected along the central axis pipe and then flows down along the pipeline. The material is deposited on the filter plate and repeatedly filtered and washed by the material pump of the circulating centrifugal pump to achieve the washing and filtering effect. When the washing end point is reached, the water in the reactor is emptied, and the high-speed stirring and shaking are started and stopped by inching. The filter cake settled on the perforated plate filter cloth is thrown off and collected in the storage tank through the discharge port at the bottom of the washing kettle. In the washing process, the nitrogen bubbling at the lower left end can not only play a stirring role, but also carry ammonia into the gas phase pipeline. The number of the filter plates is 8-15 (adjusted according to the height of the reactor), the diameter of the dense pores of the filter plates is 8-15 mm, the number of filter cloths is 1000-4000 meshes, and the conductivity of the filtrate at the end of washing is 50-300 us / cm.
[0014] D. Middle of the washing kettle: There is an observation hole in the middle of the washing kettle
[0015] E. Lower part of washing kettle: There is a nitrogen inlet valve at the lower left end of the washing kettle to purge ammonia in the filter cake. Nitrogen is blown by bubbling, and the blowing rate is 10ml-60ml / min. There is a pneumatic pump at the lower right end of the washing kettle to circulate washing water. There is a drain valve and a solid discharge port at the bottom of the washing kettle.
[0016] Furthermore, an efficient and safe EG catalyst cleaning method includes the following steps:
[0017] A. Grinding: Grinding by two grinding balls connected to each other;
[0018] B. Filtration: After the liquid particle size reaches the standard after grinding, it flows out through the filter and flows into the washing kettle along the pipeline. The size of the stainless steel filter is 1-10um. The processing capacity of the ball mill is 50-300kg / min; the temperature of the hot water tank is 0-100℃;
[0019] C. Washing: The materials flowing into the washing kettle are filtered on the mesh plate, and the permeated water is collected along the central axis pipe and then flows down along the pipeline;
[0020] D. Bubbling: The nitrogen bubbling at the lower left end can not only play a stirring role, but also carry ammonia into the gas phase pipeline;
[0021] E. Tail gas collection: Ammonia gas purged by nitrogen enters the spray tower, and the spray centrifugal pump carries out water spraying circulation. There is water at the bottom of the spray tower kettle. The residual gas at the upper end of the spray tower enters the gas-liquid separator to separate the liquid and is stored in the storage tank together with the ammonia water in the spray tower. The upper end of the gas-liquid separator is connected to a vacuum pump to extract negative pressure;
[0022] F. After the washed material enters the drying box through the conveyor belt, the dried material is stored in the storage tank, where the drying temperature is 60-150℃.
[0023] Example 1
[0024] The reaction wet material is 6 tons, the ball mill processing capacity is 100kg / min (the pore size of the outlet filter of the ball mill is 6um), the temperature in the washing kettle is maintained at 60℃, the vacuum degree of the vacuum pump is -0.2, the nitrogen bubbling flow rate is 60ml / min, there are 10 filter discs in the washing kettle with a diameter of 10mm, the number of filter cloths is 4000 mesh, and the conductivity at the washing end point is 120us / cm.
[0025] The EG catalyst is prepared by precipitation method. When the reaction end point is reached, 6t of EG reaction material (temperature 60℃) flows into the wet ball mill. After grinding, the material with a particle size of ≤5um passes through a wire filter (aperture 6um) and is mixed with hot water and flows into the washing kettle. The total liquid volume of the washing kettle is controlled to be 2 / 3 of the washing kettle, and the processing capacity of the ball mill is 100kg / min. Then, the material is stirred to mix and vacuum pump filtration and washing are carried out. After the conductivity of the filtrate after washing is ≤120us / cm, the liquid in the reactor is further vacuum-drained and the water at the bottom of the washing kettle is discharged. Material collection stage: Turn on high-speed stirring, throw off the filter cake settled on the filter plate and collect it in the storage tank. After the obtained filter cake is dried at 120℃ on a conveyor belt, it is pressed into tablets and evaluated.
[0026] Evaluation conditions: reaction temperature 190℃, 3MPa, V(H2)=80ml / min, WHSV=0.2h-1, n(H2) / n(DMO)=100(mol / mol)
[0027] Example 2
[0028] The reaction wet material is 6 tons, the ball mill processing capacity is 100kg / min (the outlet filter mesh of the ball mill has an aperture of 10um), the temperature in the washing kettle is maintained at 60℃, the vacuum degree of the vacuum pump is -0.2, the nitrogen bubbling flow rate is 60ml / min, there are 10 suction filter discs in the washing kettle, the diameter is 10mm, the number of filter cloths is 4000 mesh, and the conductivity at the washing end point is about 120us / cm. Others are the same
[0029] Example 3
[0030] The reaction wet material is 6 tons, the ball mill processing capacity is 100kg / min (the outlet filter mesh of the ball mill has an aperture of 3um), the temperature in the washing kettle is maintained at 60℃, the vacuum degree of the vacuum pump is -0.2, the nitrogen bubbling flow rate is 60ml / min, there are 10 suction filter discs in the washing kettle, the diameter is 10mm, the number of filter cloths is 4000 mesh, and the conductivity at the washing end point is about 120us / cm. Others are the same
[0031] Example 4
[0032] The reaction wet material is 6 tons, the ball mill processing capacity is 100kg / min (the outlet filter mesh of the ball mill has an aperture of 6um), the temperature in the washing kettle is maintained at 80℃, the vacuum degree of the vacuum pump is -0.2, the nitrogen bubbling flow rate is 60ml / min, there are 10 suction filter discs in the washing kettle, the diameter is 10mm, the number of filter cloths is 4000 mesh, and the conductivity at the washing end point is about 120us / cm. Others are the same
[0033] Example 5
[0034] The reaction wet material is 6 tons, the ball mill processing capacity is 100kg / min (the outlet filter mesh of the ball mill has an aperture of 6um), the temperature in the washing kettle is maintained at 40℃, the vacuum degree of the vacuum pump is -0.2, the nitrogen bubbling flow rate is 60ml / min, there are 10 suction filter discs in the washing kettle, the diameter is 10mm, the number of filter cloths is 4000 meshes, and the conductivity at the washing end point is about 120us / cm. Others are the same.
[0035] Example 6
[0036] The reaction wet material is 6 tons, the ball mill processing capacity is 100kg / min (the outlet filter mesh of the ball mill has an aperture of 6um), the temperature in the washing kettle is maintained at 60℃, the vacuum degree of the vacuum pump is -0.2, the nitrogen bubbling flow rate is 60ml / min, there are 10 suction filter discs in the washing kettle, the diameter is 10mm, the number of filter cloths is 4000 mesh, and the conductivity at the washing end point is about 200us / cm. Others are the same
[0037] Example 7
[0038] The reaction wet material is 6 tons, the ball mill processing capacity is 100kg / min (the outlet filter mesh of the ball mill has an aperture of 6um), the temperature in the washing kettle is maintained at 60℃, the vacuum degree of the vacuum pump is -0.2, the nitrogen bubbling flow rate is 60ml / min, there are 10 suction filter discs in the washing kettle, the diameter is 10mm, the number of filter cloths is 4000 meshes, and the conductivity at the washing end point is about 50us / cm. Others are the same.
[0039] Characterization and evaluation data analysis
[0040] The characterization and single tube evaluation experiment was carried out under the evaluation conditions of reaction temperature 190℃, 3MPa, V(H2)=80ml / min, WHSV=1.8h-1, n(H2) / n(DMO)=100(mol / mol).
[0041] (1) Physical properties of EG finished products
[0042] Example 1: Bulk density g / ml: 0.46, powder particle size D50 um: 53, specific surface area m2 / g: 350;
[0043] Example 2: Bulk density g / ml: 0.54, powder particle size D50 um: 62, specific surface area m2 / g: 314;
[0044] Example 3: Bulk density g / ml: 0.41, powder particle size D50 um: 46, specific surface area m2 / g: 368;
[0045] Example 4: Bulk density g / ml: 0.47, powder particle size D50 um: 52, specific surface area m2 / g: 341
[0046] Example 5: Bulk density g / ml: 0.45, powder particle size D50 um: 48, specific surface area m2 / g: 361
[0047] Example 6: Bulk density g / ml: 0.50, powder particle size D50 um: 51, specific surface area m2 / g: 345
[0048] Example 7: Bulk density g / ml: 0.48, powder particle size D50 um: 48, specific surface area m2 / g: 355.
[0049] Assessment data analysis
[0050] Experiment 1: Con (DMO): 100, Se l (EG): 97.2, Se l (MG): 0.5, Se l (BDO): 1.36, Se l (ET): 0.45, Se l (Others): 0.49, reactor temperature ℃: 170
[0051] Experiment 2: Con (DMO): 100, Se l (EG): 96.2, Se l (MG): 0.72, Se l (BDO): 1.86, Se l (ET): 0.35, Se l (Others): 0.87, reactor temperature °C: 178
[0052] Experiment 3: Con (DMO): 100, Se l (EG): 97.79, Se l (MG): 0.44, Se l (BDO): 1.08, Se l (ET): 0.36, Se l (Others): 0.33, reactor temperature °C: 166
[0053] Experiment 4: Con (DMO): 100, Se l (EG): 95.92, Se l (MG): 0.81, Se l (BDO): 1.85, Se l (ET): 0.56, Se l (Others): 0.86, reactor temperature °C: 186
[0054] Experiment 5: Con (DMO): 100, Se l (EG): 98.1, Se l (MG): 0.34, Se l (BDO): 0.97, Se l (ET): 0.33, Se l (Others): 0.26, reactor temperature °C: 162
[0055] Experiment 6: Con (DMO): 100, Se l (EG): 94.6, Se l (MG): 0.8, Se l (BDO): 2.11, Se l (ET): 0.75, Se l (Others): 1.74, reactor temperature °C: 186
[0056] Experiment 7: Con (DMO): , Se l (EG): 98.5, Se l (MG): 0.3, Se l (BDO): 0.76, Se l (ET): 0.25, Se l (Others): 0.19, reactor temperature ℃: 160. BRIEF DESCRIPTION OF THE DRAWINGS
[0057] Figure 1 The physical properties of the finished product of an efficient and safe EG catalyst cleaning method and device proposed by the present invention are characterized;
[0058] Figure 2 The evaluation data analysis of an efficient and safe EG catalyst cleaning method and device proposed by the present invention;
[0059] Figure 3 This is an overall diagram of an efficient and safe EG catalyst cleaning method and device proposed by the present invention;
[0060] Figure 4 This is a schematic diagram of a filtration plate of an efficient and safe EG catalyst cleaning method and device proposed by the present invention. DETAILED DESCRIPTION
[0061] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.
[0062] In the description of the present invention, it is necessary to understand that the terms "upper", "lower", "front", "back", "left", "right", "top", "bottom", "inside", "outside", etc., indicating the orientation or position relationship are based on the orientation or position relationship shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention.
[0063] Reference Figure 1-4 , an efficient and safe EG catalyst cleaning method and device, including a wet ball mill, a washing kettle, a hot water tank, a spray tower, a spray centrifugal pump, a gas-liquid separator, a vacuum pump, an ammonia water collection tank, a circulating centrifugal pump, a conveyor belt and a drying box;
[0064] The wet ball mill device includes a material connected to the ball mill, the lower end of the ball mill discharge port is connected to the lower end of the hot water tank pipe and flows into the washing kettle, wherein the ball mill is composed of two grinding balls connected to each other, and the lower end of the ball mill is a stainless steel filter. When the liquid particle size reaches the standard after grinding, it flows out through the filter and flows into the washing kettle along the pipeline, wherein the size of the stainless steel filter is 1-10um. The processing capacity of the ball mill is 50-300kg / min; the temperature of the hot water tank is 0-100℃;
[0065] The outer wall of the washing kettle is insulated by a steam jacket, the steam temperature in the jacket is 0-200°C, and it is heated by an annular steam pipe, and a temperature controller is installed inside, wherein the constant temperature required for the washing process is 30-80°C, a feed port with a valve is arranged at the upper end of the outer side of the washing kettle, a pipe port is arranged for the material filtered from the filter screen after grinding and mixed with hot water, a gas phase pipe is connected to the upper part of the right outer end of the washing kettle, a circular suction filter disc is arranged inside the washing kettle, the suction filter disc is made of thickened stainless steel, the orifice plate disc is funnel-shaped, a plurality of suction filter discs are arranged, a filter cloth is laid on the suction filter disc, an axial tube is arranged at the center of the suction filter disc, the axial tube is connected to each suction filter disc from top to bottom, and the axial tube is connected to a high-speed stirrer, a circulating centrifugal pump used in conjunction with the washing kettle is installed on one side of the washing kettle, an observation hole is arranged in the middle of the washing kettle, a nitrogen inlet valve is arranged at the lower left end of the washing kettle, a pneumatic pump is connected to the lower end of the washing kettle, and a drain valve and a solid discharge port are arranged at the lowest end of the washing kettle.
[0066] Hot water tank-wet grinder device
[0067] The material is connected to the ball mill feeder, and the lower end of the ball mill outlet is connected to the lower end of the hot water tank pipe and flows into the washing kettle. The ball mill has two grinding balls connected to each other for grinding. The lower end of the ball mill is a stainless steel filter. When the liquid particle size reaches the standard after grinding, it flows out through the filter and flows into the washing kettle along the pipeline. The size of the stainless steel filter is 1-10um. The processing capacity of the ball mill is 50-300kg / min; the temperature of the hot water tank is 0-100℃;
[0068] ②Composition of two washing kettles
[0069] A. The outer wall of the washing kettle is insulated with a steam jacket. The steam temperature in the jacket is 0-200℃, and it is heated by an annular steam pipe with a built-in temperature controller. The constant temperature required for the washing process is 30-80℃.
[0070] B. The upper outer side of the washing kettle: one of the feed ports has a valve, and the material filtered by the filter is mixed with hot water and then flows out of the pipe; the upper right outer end is connected to a gas phase pipe for discharge.
[0071] C. Working principle of the internal circular filter plate of the washing kettle: It is composed of multiple thickened stainless steel perforated discs, shaped like a Büchner funnel without a flat edge, and a filter cloth is laid on the top of the perforated plate. The center of the filter plate is connected by a central axis pipe from the first filter plate to the bottom layer. The central axis pipe is controlled by a high-speed agitator. The material flowing into the washing kettle is filtered on the mesh plate, and the permeated water is collected along the central axis pipe and then flows down along the pipeline. The material is deposited on the filter plate and repeatedly filtered and washed by the material pump of the circulating centrifugal pump to achieve the washing and filtering effect. When the washing end point is reached, the water in the reactor is emptied, and the high-speed stirring and shaking are started and stopped by inching. The filter cake settled on the perforated plate filter cloth is thrown off and collected in the storage tank through the discharge port at the bottom of the washing kettle. In the washing process, the nitrogen bubbling at the lower left end can not only play a stirring role, but also carry ammonia into the gas phase pipeline. The number of the filter plates is 8-15 (adjusted according to the height of the reactor), the diameter of the dense pores of the filter plates is 8-15 mm, the number of filter cloths is 1000-4000 meshes, and the conductivity of the filtrate at the end of washing is 50-300 us / cm.
[0072] D. Middle of the washing kettle: There is an observation hole in the middle of the washing kettle
[0073] E. Lower part of washing kettle: There is a nitrogen inlet valve at the lower left end of the washing kettle for blowing ammonia in the filter cake. Nitrogen is blown by bubbling, and the blowing rate is 10ml-60ml / min. A pneumatic pump is connected to the lower right end of the washing kettle for circulating washing water. There is a drain valve and a solid discharge port at the bottom of the washing kettle. Further, an efficient and safe EG catalyst cleaning method includes the following steps:
[0074] A. Grinding: Grinding by two grinding balls connected to each other;
[0075] B. Filtration: After the liquid particle size reaches the standard after grinding, it flows out through the filter and flows into the washing kettle along the pipeline. The size of the stainless steel filter is 1-10um. The processing capacity of the ball mill is 50-300kg / min; the temperature of the hot water tank is 0-100℃;
[0076] C. Washing: The materials flowing into the washing kettle are filtered on the mesh plate, and the permeated water is collected along the central axis pipe and then flows down along the pipeline;
[0077] D. Bubbling: The nitrogen bubbling at the lower left end can not only play a stirring role, but also carry ammonia into the gas phase pipeline;
[0078] E. Tail gas collection: Ammonia gas purged by nitrogen enters the spray tower, and the spray centrifugal pump carries out water spraying circulation. There is water at the bottom of the spray tower kettle. The residual gas at the upper end of the spray tower enters the gas-liquid separator to separate the liquid and is stored in the storage tank together with the ammonia water in the spray tower. The upper end of the gas-liquid separator is connected to a vacuum pump to extract negative pressure;
[0079] F. After the washed material enters the drying box through the conveyor belt, the dried material is stored in the storage tank, where the drying temperature is 60-150℃.
[0080] Example 1
[0081] The reaction wet material is 6 tons, the ball mill processing capacity is 100kg / min (the pore size of the outlet filter of the ball mill is 6um), the temperature in the washing kettle is maintained at 60℃, the vacuum degree of the vacuum pump is -0.2, the nitrogen bubbling flow rate is 60ml / min, there are 10 filter discs in the washing kettle with a diameter of 10mm, the number of filter cloths is 4000 mesh, and the conductivity at the washing end point is 120us / cm.
[0082] The EG catalyst is prepared by precipitation method. When the reaction end point is reached, 6t of EG reaction material (temperature 60℃) flows into the wet ball mill. After grinding, the material with a particle size of ≤5um passes through a wire filter (aperture 6um) and is mixed with hot water and flows into the washing kettle. The total liquid volume of the washing kettle is controlled to be 2 / 3 of the washing kettle, and the processing capacity of the ball mill is 100kg / min. Then, the material is stirred to mix and vacuum pump filtration and washing are carried out. After the conductivity of the filtrate after washing is ≤120us / cm, the liquid in the reactor is further vacuum-drained and the water at the bottom of the washing kettle is discharged. Material collection stage: Turn on high-speed stirring, throw off the filter cake settled on the filter plate and collect it in the storage tank. After the obtained filter cake is dried at 120℃ on a conveyor belt, it is pressed into tablets and evaluated.
[0083] Evaluation conditions: reaction temperature 190℃, 3MPa, V(H2)=80ml / min, WHSV=0.2h-1, n(H2) / n(DMO)=100(mol / mol)
[0084] Example 2
[0085] The reaction wet material is 6 tons, the ball mill processing capacity is 100kg / min (the outlet filter mesh of the ball mill has an aperture of 10um), the temperature in the washing kettle is maintained at 60℃, the vacuum degree of the vacuum pump is -0.2, the nitrogen bubbling flow rate is 60ml / min, there are 10 suction filter discs in the washing kettle, the diameter is 10mm, the number of filter cloths is 4000 mesh, and the conductivity at the washing end point is about 120us / cm. Others are the same
[0086] Example 3
[0087] The reaction wet material is 6 tons, the ball mill processing capacity is 100kg / min (the outlet filter mesh of the ball mill has an aperture of 3um), the temperature in the washing kettle is maintained at 60℃, the vacuum degree of the vacuum pump is -0.2, the nitrogen bubbling flow rate is 60ml / min, there are 10 suction filter discs in the washing kettle, the diameter is 10mm, the number of filter cloths is 4000 mesh, and the conductivity at the washing end point is about 120us / cm. Others are the same
[0088] Example 4
[0089] The reaction wet material is 6 tons, the ball mill processing capacity is 100kg / min (the outlet filter mesh of the ball mill has an aperture of 6um), the temperature in the washing kettle is maintained at 80℃, the vacuum degree of the vacuum pump is -0.2, the nitrogen bubbling flow rate is 60ml / min, there are 10 suction filter discs in the washing kettle, the diameter is 10mm, the number of filter cloths is 4000 mesh, and the conductivity at the washing end point is about 120us / cm. Others are the same
[0090] Example 5
[0091] The reaction wet material is 6 tons, the ball mill processing capacity is 100kg / min (the outlet filter mesh of the ball mill has an aperture of 6um), the temperature in the washing kettle is maintained at 40℃, the vacuum degree of the vacuum pump is -0.2, the nitrogen bubbling flow rate is 60ml / min, there are 10 suction filter discs in the washing kettle, the diameter is 10mm, the number of filter cloths is 4000 meshes, and the conductivity at the washing end point is about 120us / cm. Others are the same.
[0092] Example 6
[0093] The reaction wet material is 6 tons, the ball mill processing capacity is 100kg / min (the outlet filter mesh of the ball mill has an aperture of 6um), the temperature in the washing kettle is maintained at 60℃, the vacuum degree of the vacuum pump is -0.2, the nitrogen bubbling flow rate is 60ml / min, there are 10 suction filter discs in the washing kettle, the diameter is 10mm, the number of filter cloths is 4000 mesh, and the conductivity at the washing end point is about 200us / cm. Others are the same
[0094] Example 7
[0095] The reaction wet material is 6 tons, the ball mill processing capacity is 100kg / min (the outlet filter mesh of the ball mill has an aperture of 6um), the temperature in the washing kettle is maintained at 60℃, the vacuum degree of the vacuum pump is -0.2, the nitrogen bubbling flow rate is 60ml / min, there are 10 suction filter discs in the washing kettle, the diameter is 10mm, the number of filter cloths is 4000 meshes, and the conductivity at the washing end point is about 50us / cm. Others are the same.
[0096] Characterization and evaluation data analysis
[0097] The characterization and single tube evaluation experiment was carried out under the evaluation conditions of reaction temperature 190℃, 3MPa, V(H2)=80ml / min, WHSV=1.8h-1, n(H2) / n(DMO)=100(mol / mol).
[0098] (1) Physical properties of EG finished products
[0099] Example 1: Bulk density g / ml: 0.46, powder particle size D50 um: 53, specific surface area m2 / g: 350;
[0100] Example 2: Bulk density g / ml: 0.54, powder particle size D50 um: 62, specific surface area m2 / g: 314;
[0101] Example 3: Bulk density g / ml: 0.41, powder particle size D50 um: 46, specific surface area m2 / g: 368;
[0102] Example 4: Bulk density g / ml: 0.47, powder particle size D50 um: 52, specific surface area m2 / g: 341
[0103] Example 5: Bulk density g / ml: 0.45, powder particle size D50 um: 48, specific surface area m2 / g: 361
[0104] Example 6: Bulk density g / ml: 0.50, powder particle size D50 um: 51, specific surface area m2 / g: 345
[0105] Example 7: Bulk density g / ml: 0.48, powder particle size D50 um: 48, specific surface area m2 / g: 355.
[0106] Assessment data analysis
[0107] Experiment 1: Con (DMO): 100, Se l (EG): 97.2, Se l (MG): 0.5, Se l (BDO): 1.36, Se l (ET): 0.45, Se l (Others): 0.49, reactor temperature ℃: 170
[0108] Experiment 2: Con (DMO): 100, Se l (EG): 96.2, Se l (MG): 0.72, Se l (BDO): 1.86, Se l (ET): 0.35, Se l (Others): 0.87, reactor temperature °C: 178
[0109] Experiment 3: Con (DMO): 100, Se l (EG): 97.79, Se l (MG): 0.44, Se l (BDO): 1.08, Se l (ET): 0.36, Se l (Others): 0.33, reactor temperature °C: 166
[0110] Experiment 4: Con (DMO): 100, Se l (EG): 95.92, Se l (MG): 0.81, Se l (BDO): 1.85, Se l (ET): 0.56, Se l (Others): 0.86, reactor temperature °C: 186
[0111] Experiment 5: Con (DMO): 100, Se l (EG): 98.1, Se l (MG): 0.34, Se l (BDO): 0.97, Se l (ET): 0.33, Se l (Others): 0.26, reactor temperature °C: 162
[0112] Experiment 6: Con (DMO): 100, Se l (EG): 94.6, Se l (MG): 0.8, Se l (BDO): 2.11, Se l (ET): 0.75, Se l (Others): 1.74, reactor temperature °C: 186
[0113] Experiment 7: Con (DMO): , Se l (EG): 98.5, Se l (MG): 0.3, Se l (BDO): 0.76, Se l (ET): 0.25, Se l (Others): 0.19, reactor temperature ℃: 160.
[0114] The above are only preferred specific implementation modes of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical solutions and inventive concepts of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.
Claims
1. An efficient and safe EG catalyst cleaning device, characterized in that: It includes a wet ball mill, a washing kettle, a hot water tank, a spray tower, a spray centrifugal pump, a gas-liquid separator, a vacuum pump, an ammonia water collection tank, a circulating centrifugal pump, a conveyor belt and a drying box; The wet ball mill device includes a material connected to a ball mill, the lower end of the ball mill outlet is connected to the lower end of the hot water tank pipe and flows into the washing kettle, wherein the ball mill is composed of two mutually connected grinding balls, and the lower end of the ball mill is a stainless steel filter; The outer wall of the washing kettle is insulated by a steam jacket, the steam temperature in the jacket is 0-200°C, and it is heated by an annular steam pipe, wherein the constant temperature required for the washing process is 30-80°C, a feed port with a valve is arranged at the upper end of the outer side of the washing kettle, a gas phase pipe is connected to the upper part of the right outer end of the washing kettle, a circular suction filter disk is arranged inside the washing kettle, the suction filter disk is made of thickened stainless steel, the orifice plate disk is funnel-shaped, a plurality of suction filter disks are arranged, a filter cloth is laid on the suction filter disk, an axial tube is arranged at the center of the suction filter disk, the axial tube is connected to each suction filter disk from top to bottom, the axial tube is connected to a high-speed agitator, a circulating centrifugal pump used in conjunction with the washing kettle is installed on one side of the washing kettle, an observation hole is arranged in the middle of the washing kettle, a nitrogen inlet valve is arranged at the lower left end of the washing kettle, a pneumatic pump is connected to the lower end of the washing kettle, and a drain valve and a solid discharge port are arranged at the lowest end of the washing kettle.
2. An efficient and safe EG catalyst cleaning method according to claim 1, characterized in that: The steps include: A. Grinding: Grinding by two interlocking grinding balls; B. Filtration: After the liquid particle size reaches the standard after grinding, it flows out through the filter and flows into the washing kettle along the pipeline. The size of the stainless steel filter is 1-10um. The processing capacity of the ball mill is 50-300kg / min; the temperature of the hot water tank is 0-100℃; C. Washing: The materials flowing into the washing kettle are filtered on the mesh plate, and the permeated water is collected along the central axis pipe and then flows down along the pipeline; D. Bubbling: The nitrogen bubbling at the lower left end can not only play a stirring role, but also carry ammonia into the gas phase pipeline; E. Tail gas collection: Ammonia gas purged by nitrogen enters the spray tower, and the spray centrifugal pump carries out water spraying circulation. There is water at the bottom of the spray tower kettle. The residual gas at the upper end of the spray tower enters the gas-liquid separator to separate the liquid and is stored in the storage tank together with the ammonia water in the spray tower. The upper end of the gas-liquid separator is connected to a vacuum pump to extract negative pressure; F. After the washed material enters the drying box through the conveyor belt, the dried material is stored in the storage tank, where the drying temperature is 60-150℃.