CN115228381A - Loading construction method of supported catalyst - Google Patents
Loading construction method of supported catalyst Download PDFInfo
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- CN115228381A CN115228381A CN202210736392.2A CN202210736392A CN115228381A CN 115228381 A CN115228381 A CN 115228381A CN 202210736392 A CN202210736392 A CN 202210736392A CN 115228381 A CN115228381 A CN 115228381A
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- reactor
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- filling
- purging
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- 239000003054 catalyst Substances 0.000 title claims abstract description 75
- 238000010276 construction Methods 0.000 title claims abstract description 27
- 238000005488 sandblasting Methods 0.000 claims abstract description 26
- 238000010926 purge Methods 0.000 claims abstract description 24
- 238000004140 cleaning Methods 0.000 claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000007789 sealing Methods 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000000694 effects Effects 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 18
- 238000012360 testing method Methods 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 238000005507 spraying Methods 0.000 claims description 12
- 239000004576 sand Substances 0.000 claims description 11
- 238000007689 inspection Methods 0.000 claims description 9
- 238000007599 discharging Methods 0.000 claims description 4
- 238000009423 ventilation Methods 0.000 claims description 4
- 239000006004 Quartz sand Substances 0.000 claims description 3
- 238000013461 design Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 239000002699 waste material Substances 0.000 claims description 3
- 238000009434 installation Methods 0.000 claims description 2
- 238000012797 qualification Methods 0.000 abstract description 4
- 230000003749 cleanliness Effects 0.000 abstract description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 8
- 229910052709 silver Inorganic materials 0.000 description 8
- 239000004332 silver Substances 0.000 description 8
- 239000000428 dust Substances 0.000 description 7
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 5
- 239000003086 colorant Substances 0.000 description 5
- 238000005422 blasting Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000007664 blowing Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 2
- 238000005429 filling process Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- CCGKOQOJPYTBIH-UHFFFAOYSA-N ethenone Chemical compound C=C=O CCGKOQOJPYTBIH-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000000474 nursing effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 229940100890 silver compound Drugs 0.000 description 1
- 150000003379 silver compounds Chemical class 0.000 description 1
- -1 silver ketene) Chemical class 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
- B01J8/002—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor with a moving instrument
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention relates to a loading construction method of a supported catalyst, wherein a weather enclosure is erected at the top of a reactor before loading, the reactor is injected with water to build circulating temperature rise, sand blasting is carried out on a tube array to be loaded with the catalyst by adopting sand blasting equipment, zone identification and zone division are carried out on the reactor, sponge balls are numbered and plugged into the tube array of the reactor, a purging gun is plugged into the tube array, the head of the purging gun is made of soft tapered rubber, a sealing effect is formed after the purging gun is plugged, an air valve is opened to introduce gas, and the sponge balls are discharged from top to bottom, so that the purpose of cleaning the tube array is achieved; cleaning the regions by using sponge balls, and replacing one region after one region is hit; and filling a catalyst after the spring at the bottom of the reactor is installed, measuring the altitude, purging and pressure difference, installing a thermocouple, and sealing with nitrogen. The invention improves the filling qualification rate by controlling the temperature, the humidity, the cleanliness and the like of the reactor, and prolongs the running period of the catalyst.
Description
Technical Field
The invention relates to a catalyst filling construction method, in particular to a shell and tube type loading catalyst filling construction method.
Background
In BOf the olefinic downstream derivatives, ethylene oxide/ethylene glycol (EO/EG) is still a rapidly growing industry, particularly in china and the middle east. Silver catalyst has been developed in 1930 and is used as the only catalyst for ethylene oxide production by ethylene oxidation. The catalyst is generally alpha-Al 2 O 3 As carrier, the silver content is 10-30%. In order to improve the performance of the catalyst, promoters such as rubidium, cesium, calcium, barium and the like are often added. Typically prepared by impregnating Al with a silver nitrate solution 2 O 3 The carrier is then thermally decomposed to produce the catalyst. Later, it was found that by re-decomposing an organic silver compound (such as silver ketene), a catalyst with finer silver grains and better dispersion can be prepared, and the selectivity is greatly improved. In addition, the carrier silver catalyst is also used as a catalytic electrode (Ag/active carbon) of a fuel cell and for producing p-xylene (Ag/Al) by toluene disproportionation in petrochemical industry 2 O 3 )。
The main structure of the ethylene oxide reactor is as follows: the shell, the tube bundle, the tube plate, the support grid, the upper end enclosure and the lower end enclosure are internally provided with tens of thousands of reaction tubes, so that the correct loading construction of the supported silver catalyst is particularly important for ensuring the high selectivity of the silver catalyst, and the strict requirements on the loading height, compactness and the temperature, humidity and cleanliness of a reactor are met in the catalyst loading process.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a loading construction method of a supported catalyst, which can improve the loading qualification rate.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a loading construction method of a supported catalyst comprises the following steps:
step one, construction preparation
A rainproof shed is erected at the top of the reactor, water is injected into the reactor to establish circulating temperature rise, and the temperature in the reactor is higher than the ambient temperature by 40 +/-5 ℃;
step two, column Guan Pensha cleaning
Carrying out sand blasting treatment on the tubes to be filled with the catalyst by adopting sand blasting equipment, determining 3-5 test tubes before sand blasting, and carrying out test sand blasting on the first test tube; using an endoscope to check the trial spraying result, adjusting trial spraying parameters, performing trial spraying and inspection on other test tubes, and determining the parameters of formal sand spraying according to the inspection result;
step three, sponge ball cleaning
Carrying out zone identification and zone division on the reactor, numbering sponge balls in the zone division by taking 10 columns as a zone, plugging the sponge balls into the reactor tubes, plugging a purging gun into the tubes, wherein the gun head of the purging gun is made of soft tapered rubber, forming a sealing effect after plugging the purging gun, opening an air valve, introducing gas, and discharging the sponge balls from top to bottom to achieve the purpose of cleaning the tubes; cleaning the regions by using sponge balls, and replacing one region after one region is hit;
step four, installing a bottom spring
Loading the spring into the tube array until the spring is limited, wherein the spring loading process follows the area division of the step three;
step five, filling the catalyst
Filling according to the area divided in the third step, and measuring and adjusting the height of the filled tube array to meet the design value of the filling height of the catalyst; the reactor interior was kept dry during the filling period;
step six, measuring altitude, purging and pressure difference;
step seven, installing a thermocouple and sealing nitrogen
And installing a thermocouple, connecting the inlet and the outlet of the reactor, flushing nitrogen for protection after the connection is finished, and raising the temperature of the reactor according to the technical requirements.
Further, in the first step, a temporary catalyst storage canopy is erected on the ground; after the reactor is opened, a scaffold platform required by the operation of a lower end enclosure of the reactor is set up, a straight ladder entering the reactor is prepared, and the contact point of the straight ladder and a tube plate is protected in a wrapping mode.
Further, in the second step, a row-by-row sand blasting mode is adopted until all the steps are finished; in the sand blasting process, redundant ash and waste sand in the space of the lower end socket are pumped away by a vacuum pump.
Furthermore, in the second step, the sand used for sand blasting is dry quartz sand with the specification of 20-40 meshes and the hardness of 6-7.
Further, in the third step, the specification of the sponge ball is phi 55 x 120mm.
And further, in the fifth step, the catalyst is hoisted to the reactor platform and then poured into the filling hopper, the lower part of the filling hopper is connected with a discharge pipeline and a discharge groove, the discharge groove is connected with a suction ash removal pipeline, and when the catalyst is poured into the filling hopper, vacuum equipment connected with the suction ash removal pipeline is started for ash removal.
Further, in the sixth step, the filling height of the catalyst is detected by using a measuring ruler, the time required for blowing each reaction tube clean is confirmed, and a blowing instrument is timed to blow each reaction tube; and measuring the pressure drop by using a pressure drop measuring instrument and recording the pressure drop value of each reaction tube, wherein the pressure drop measured by different instruments of the same reaction tube is within +/-3% of the reference standard pressure drop.
Furthermore, the temperature in the reactor is higher than the highest temperature of the external environment by 5-10 ℃ during construction, the temperature of a bed layer of the reactor is strictly controlled within a range, and an air conditioner is used for ventilation.
The invention adopts sand blasting and sponge ball cleaning to make the tube array cleaner, establishes a water circulation system, keeps constant temperature and creates a better temperature environment for catalyst filling. In conclusion, by adopting the construction method provided by the invention, the temperature, the humidity, the cleanliness and the like of the reactor are controlled in the catalyst filling process, so that the filling qualification rate is improved, and the catalyst operation period is prolonged.
Detailed Description
The present embodiment is illustrated by taking a typical ethylene oxide reactor as an example, the main structure of the ethylene oxide reactor comprises a shell, a tube bundle, a tube plate, a support grid, an upper end enclosure and a lower end enclosure, the diameter of the reactor is 8065mm, the total height of the reactor is about 22538mm, and 15569 reaction tubes are arranged in the reactor. The reaction tube has an outer diameter of 50.8mm, an inner diameter of 44.8mm and a length of 9920mm. The silver catalyst loading per reactor was about 202t and the inert ball was about 26t.
A rain-proof shed is arranged at the top of the reactor to prevent rainwater and dust from entering the reactor. The reactor is prevented from being cleaned and filled with the catalyst in rainy days. The reactor is injected with water to build up circulating temperature rise, and the temperature in the reactor must be higher than the ambient temperature by about 40 ℃ to avoid rusting due to moisture. Good illumination and ventilation should be provided in the reactor, and the temporary power supply of all the tools must be provided with an electric leakage protection device to ensure safety.
Preparation for construction
The construction scheme is compiled before the construction is started, personnel are organized, technical background is carried out, meanwhile, the test before filling is carried out, the actual filling height and the filling compactness are determined to be consistent with the requirement of the scheme, and the standard is used for quality acceptance in the whole construction process.
And (3) erecting a temporary catalyst storage canopy on the ground, and erecting a platform operation canopy before opening the reactor to ensure the qualification. After the reactor is opened, a scaffold platform required by lower end enclosure operation is erected, a straight ladder entering the reactor is prepared, and the straight ladder needs to be protected in a wrapping mode at a tube plate contact point.
To ensure the reactor is dry, the loading quality of the catalyst is ensured. A heat removing agent system is utilized to establish a water circulation system, the temperature in the reactor is 5-10 ℃ higher than the highest temperature of the external environment during construction, the temperature of a bed layer of the reactor is strictly controlled within a range, and an air conditioner is used for ventilation.
Any articles that may fall into the array must not enter the reactor, prohibiting articles from being brought into the reactor independent of catalyst loading.
Blasting cleaning of pipe array by sand blasting
The upper and lower parts of the tube array are all covered with yellow tube caps. The sand blasting equipment is well debugged, and the air source pressure is 7barg. The sand used for sand blasting is dry refined quartz sand with the specification of 20-40 meshes and the hardness of 6-7.
The interior of the tube was examined endoscopically and 5 test tubes were identified. And setting the experiment time and the sand amount according to the construction experience, and performing test sand blasting on the first test tube. And (5) adjusting the test spraying parameters by using the endoscope examination test spraying result, and carrying out test spraying and examination on the second and the third test tubes. And determining the parameters of the formal sand blasting and inspecting the standard pipe according to the inspection result.
And removing a row of pipe caps, blasting sand one by one according to set parameters, inspecting a row of electric torches after spraying, covering the pipe caps after confirming that the standard is met, and adjusting the sand blasting parameters in time if the standard has obvious deviation. And (4) blasting sand row by row according to the method until all the sand blasting is finished. In the sand blasting process, redundant ash and waste sand in the space of the lower end enclosure are pumped away by a vacuum pump.
The caps were opened row by row, all tubes were carefully inspected with a flashlight, and the tubes that needed to be re-sprayed and damaged were marked separately. And selecting proper sand blasting parameters for the tubes needing to be re-blasted, and re-blasting once.
And after all the lower seal heads and the tube plates are inspected to be qualified, cleaning the lower seal heads and the tube plates completely. Wait for reactor shell Cheng Shiya and check all the tube arrays for leaks with a torch inside and lower nozzles.
Sponge ball cleaning
The waterproof cloth is laid on the platform at the bottom of the reactor to plug all gaps, and the bottom access area is temporarily sealed during operation, so that the whole bottom is in a completely sealed state.
The reactor is subjected to zone identification and zone division, and the division is performed throughout the whole operation process and can be used as a reference standard value for later replacement. The area division is one area per 10 columns.
Sponge balls (specification phi 55 x 120mm) are numbered and plugged into the reactor tubes, and high density sponge balls are used to prevent the sponge balls from being broken during the purging process, and the broken pieces are adsorbed on the tube walls.
The purging gun is plugged into the tube nest, the head of the purging gun is made of soft conical rubber, a sealing effect is formed after the purging gun is plugged, an air valve is opened, introduced gas is larger than 4bar, and the sponge ball is discharged from top to bottom, so that the purpose of cleaning the tube nest is achieved.
The cleaning effect was checked using an endoscope. And cleaning by using sponge balls in different areas, replacing one sponge ball after hitting one area, simultaneously checking whether the sponge balls and the tubulations in the previous area are particularly unclean, and finding out the corresponding tubulations according to positioning and numbering. After all the cleaning is finished, the sponge balls at the bottom are collected, meanwhile, the lamps are lighted at the bottom, and error-free inspection is carried out for 2 times according to the region from the upper part. After the inspection, all the tubes are covered with tube caps, and the following special emphasis is needed: all the subsequent processes are the process of replacing the tube caps, the opening of the tube openings is strictly forbidden, all the open tubes are temporarily regarded as unqualified, the tube caps with corresponding colors can be covered again only after the confirmation, and the tubes of the lower end socket heat exchanger must be completely closed until all the work is finished.
Sequence of use of caps
15600 main colors (yellow and blue) are adopted, and 1000 auxiliary colors (red) are adopted. After the springs are installed, the bottom cover is marked and the bottom of the tube array is covered.
Bottom spring mounting
The spring is placed on the tool, pushed into the tube, the pneumatic tool is controlled to load the spring until it reaches a limit, the tool is withdrawn, the cap is closed for marking, the next loading is carried out, the loading process also follows the previous zone division. After all the filling is finished, error-free inspection is carried out for 2 times, and qualified caps with different colors are covered. And after the inspection is qualified, the lower part is closed, and any air convection at the bottom is forbidden so as not to influence the filling quality of the catalyst.
Catalyst loading
The catalyst is stacked after being delivered out of the warehouse and temporarily erected in a rain shed, a specially-assigned person is used for nursing, meanwhile, the records of catalyst filling are made, the records are used for changing the filling time of the bags, the filling quality, the catalyst types, the LOT numbers and the emptied packages, and the emptied packages are orderly stacked and correspond to the records one by one.
The catalyst is hoisted to a reactor platform and poured into a stainless steel filling hopper, a discharge pipeline and a discharge groove are connected below the filling hopper, the discharge groove also needs to be connected with a suction ash removal pipeline, the suction ash removal pipeline is connected with vacuum equipment, and the vacuum equipment is started to remove ash when the catalyst is poured into the filling hopper.
And (3) uncovering the white cover according to the area, placing module filling equipment, dividing according to the area, assembling the module filling equipment, placing the module into a tube array, waiting for catalyst to be discharged, and starting filling.
Confirming that the catalyst is filled, discharging the material from a hopper outside the reactor, enabling the catalyst to flow into a filling module, enabling the module to have vibration and ash removal functions, enabling the catalyst to automatically fall into a tube array under the vibration of the module, always ensuring that the catalyst is always in the filling module and the catalyst in the hopper on the upper layer is also always in the material.
During the filling process, the catalyst falls down into the tubes by vibration, the generated dust is also sucked away, and after a group of modules is filled, the modules are taken out, placed in other unfilled areas again and assembled according to the method. And the height of the filled tube array is measured and adjusted to meet the design value of the catalyst filling height. And performing cover replacement operation on the finished and qualified tube array.
At least 2 groups of modules are arranged in the reactor for filling, the discharge hopper is ensured to be always in a material state, after 1 group of catalysts are filled, the filling pipe is moved to the 2 nd group for filling and discharging, and no waiting time exists. The filling operation is thus performed alternately. After all the parts are pulled out, the filling height, the qualified blue cover and the unqualified red cover are measured in sequence by using a scale (PVC with calibrated height).
At the time of the end of filling, the work of uncovering and inserting the filling pipe is carried out opposite to the filling area, when the filling of one area is finished, the filling of the other area can be carried out, and the whole work is carried out continuously.
And after the catalysts are completely filled, the unqualified filling is adjusted to ensure the consistency of the filling height, and after the catalysts are completely filled, the tube plates are all blue covers.
The method is adopted for filling, the filling is uniform and compact, and the compactness is improved by 2-3% compared with the compactness of a conventional funnel method, so that the reaction selectivity is improved, the radial temperature uniformity is ensured, and the running period of the catalyst is prolonged.
Filling a top ceramic ball: according to the area division, uncovering Huang Gai, erecting a filling hopper, measuring a cup by using a measuring cup, leveling by using a steel ruler, pouring into the hopper, enabling the porcelain ball to enter the tube nest, removing the hopper, covering a white cover, and filling the next tube nest. And checking the ceramic ball filling height according to the area, and measuring whether each tube array is correctly filled or not to ensure the correct filling of the ceramic balls in each tube array.
Height, blowing and pressure difference measuring
And detecting the filling height of the catalyst by using a measuring scale, covering the qualified catalyst with a pipe cap with a specified color, and measuring the unqualified catalyst again until the qualified catalyst is qualified after being reloaded.
Debugging an instrument wind purging instrument, confirming the time required for purging each reaction tube, purging each reaction tube at regular time, and marking by tube caps with different colors to ensure that the purging is not leaked.
The pressure drop measuring instrument was calibrated in advance, the pressure drop was measured and the pressure drop value of each reaction tube was recorded. The pressure drop was measured in any 10 reaction tubes at different positions in each zone, and the average was taken after discarding the tubes that deviate by + -3% from the average and taken as the reference standard pressure drop for the reactor. And taking the plurality of pipes, measuring the pressure drop by using different pressure drop measuring instruments, and requiring that the pressure drop measured by different instruments of the same reaction pipe deviates within +/-3% of the reference standard pressure drop, otherwise, adjusting the pressure drop measuring instruments to meet the requirements.
And measuring the pressure drop one by one in sequence and making a record. In the measuring process, every 200 reaction tubes are checked once in the standard pressure drop tube so as to avoid inaccurate measurement. And (4) after the pressure drop of all the reaction tubes is confirmed to be qualified, withdrawing the pressure drop tester and the tools, and removing the dust on the upper tube plate by using a dust collector.
Thermocouple installation, nitrogen gas seal
And installing a thermocouple. The thermocouple is installed by using a crane in a matching mode, the thermocouple is prevented from being damaged in the reinstalling process, and meanwhile, the thermocouple sleeve is well protected and prevented from being damaged.
Thoroughly purging the upper and lower end enclosures and the upper and lower tube plates of the reactor once by instrument air, and then removing dust and foreign matters on the upper and lower tube plates and the upper and lower end enclosures by using a dust collector, and removing catalyst dust and foreign matters in the circulating gas inlet and outlet tubes.
Connecting the inlet and the outlet of the reactor, flushing nitrogen for protection after the connection is finished, and raising the temperature of the reactor according to the technical requirements.
Claims (8)
1. The loading construction method of the supported catalyst is characterized by comprising the following steps:
step one, construction preparation
A rainproof shed is erected at the top of the reactor, water is injected into the reactor to establish circulating temperature rise, and the temperature in the reactor is higher than the ambient temperature by 40 +/-5 ℃;
step two, cleaning the column Guan Pensha
Carrying out sand blasting treatment on the tubes to be filled with the catalyst by adopting sand blasting equipment, determining 3-5 test tubes before sand blasting, and carrying out test sand blasting on the first test tube; using an endoscope to check the trial spraying result, adjusting trial spraying parameters, performing trial spraying and inspection on other test tubes, and determining the parameters of formal sand spraying according to the inspection result;
step three, sponge ball cleaning
Carrying out zone identification and zone division on the reactor, numbering sponge balls in the zone division by taking 10 columns as a zone, plugging the sponge balls into the reactor tubes, plugging a purging gun into the tubes, wherein the gun head of the purging gun is made of soft tapered rubber, forming a sealing effect after plugging the purging gun, opening an air valve, introducing gas, and discharging the sponge balls from top to bottom to achieve the purpose of cleaning the tubes; cleaning the regions by using sponge balls, and replacing one region after one region is hit;
step four, installing a bottom spring
Loading the spring into the tube array until the spring is limited, wherein the spring loading process follows the area division of the step three;
step five, filling catalyst
Filling according to the area divided in the third step, and measuring and adjusting the height of the filled tube array to meet the design value of the filling height of the catalyst; the reactor interior was kept dry during the filling period;
step six, measuring altitude, purging and pressure difference;
step seven, thermocouple installation and nitrogen sealing
And installing a thermocouple, connecting the inlet and the outlet of the reactor, flushing nitrogen for protection after the connection is finished, and raising the temperature of the reactor according to the technical requirements.
2. The loading construction method of the supported catalyst according to claim 1, characterized in that: in the first step, a temporary catalyst storage canopy is erected on the ground; after the reactor is opened, a scaffold platform required by the operation of a lower end enclosure of the reactor is set up, a straight ladder entering the reactor is prepared, and the contact point of the straight ladder and a tube plate is protected in a wrapping mode.
3. The loading construction method of the supported catalyst according to claim 1 or 2, characterized in that: in the second step, a row-by-row sand blasting mode is adopted until all the steps are finished; in the sand blasting process, redundant ash and waste sand in the space of the lower end enclosure are pumped away by a vacuum pump.
4. The loading construction method of a supported catalyst according to claim 3, characterized in that: in the second step, the sand used for sand blasting is dry quartz sand with the specification of 20-40 meshes and the hardness of 6-7.
5. The loading construction method of a supported catalyst according to claim 1 or 4, characterized in that: in the third step, the specification of the sponge ball is phi 55 x 120mm.
6. The loading construction method of the supported catalyst according to claim 5, characterized in that: and step five, after the catalyst is hoisted to the reactor platform, the catalyst is poured into a filling hopper, a discharge pipeline and a discharge chute are connected below the filling hopper, the discharge chute is connected with a suction ash removal pipeline, and when the catalyst is poured into the filling hopper, vacuum equipment connected with the suction ash removal pipeline is started for ash removal.
7. The loading construction method of a supported catalyst according to claim 6, characterized in that: step six, detecting the filling height of the catalyst by using a measuring ruler, confirming the time required for purging each reaction tube, and purging each reaction tube by using a timing purging instrument; measuring the pressure drop by a pressure drop measuring instrument and recording the pressure drop value of each reaction tube, wherein the pressure drop measured by different instruments of the same reaction tube is within +/-3 percent of the reference standard pressure drop.
8. The loading construction method of a supported catalyst according to claim 7, characterized in that: during construction, the temperature in the reactor is 5-10 ℃ higher than the highest temperature of the external environment, the temperature of the bed layer of the reactor is strictly controlled within a range, and an air conditioner is used for ventilation.
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| CN110665441A (en) * | 2019-03-25 | 2020-01-10 | 谷育英 | Spring combination for filling catalyst for tube array type fixed bed reactor |
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| CN110665441A (en) * | 2019-03-25 | 2020-01-10 | 谷育英 | Spring combination for filling catalyst for tube array type fixed bed reactor |
Non-Patent Citations (3)
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| 余成明;李小倍;张振坤;: "三塔并联甲醇装置单塔检修总结", 中氮肥, no. 02 * |
| 解英南: "浅析环氧乙烷反应器银催化剂装填技术", 《石化技术》, no. 6, pages 1 - 2 * |
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