CN106268975A - Change furnace catalyst low-pressure heater heating process gas vulcanizing equipment and vulcanization process thereof - Google Patents

Change furnace catalyst low-pressure heater heating process gas vulcanizing equipment and vulcanization process thereof Download PDF

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Publication number
CN106268975A
CN106268975A CN201610766651.0A CN201610766651A CN106268975A CN 106268975 A CN106268975 A CN 106268975A CN 201610766651 A CN201610766651 A CN 201610766651A CN 106268975 A CN106268975 A CN 106268975A
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China
Prior art keywords
process gas
nitrogen
catalyst
vulcanization
conversion pipeline
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CN201610766651.0A
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Chinese (zh)
Inventor
祁世平
孙涌
张彦平
王耀
聂峰
黄公青
徐发淮
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Inner Mongolia Boda Chemical Co Ltd
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Inner Mongolia Boda Chemical Co Ltd
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Priority to CN201610766651.0A priority Critical patent/CN106268975A/en
Publication of CN106268975A publication Critical patent/CN106268975A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/20Sulfiding

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Heating, Cooling, Or Curing Plastics Or The Like In General (AREA)

Abstract

The present invention provides a kind of change furnace catalyst low-pressure heater heating process gas vulcanizing equipment and vulcanization process thereof.Described change furnace catalyst low-pressure heater heating process gas vulcanizing equipment includes steam heater, catalyst, nitrogen aerator and process gas conversion pipeline, described steam heater is located at by described catalyst, and described nitrogen aerator, described process gas conversion pipeline is connected with described steam heater.Change furnace catalyst low-pressure heater heating process gas vulcanizing equipment and vulcanization process thereof that the present invention provides use the process gas of gasification furnace production to carry out the method vulcanized, time saving and energy saving, vulcanize more thorough.

Description

Change furnace catalyst low-pressure heater heating process gas vulcanizing equipment and vulcanization process thereof
Technical field
The invention belongs to condenser equipment technical field, particularly relate to a kind of change furnace catalyst low-pressure heater heater Skill gas vulcanizing equipment and vulcanization process thereof.
Background technology
Traditional transformation catalyst sulfuration CS2+H2 and low-pressure heater are carried out, and it is relatively big that the method exists risk, Vulcanizing not thorough, CS2 easily accumulates in the catalyst, is easy to overtemperature after introducing technology gas simultaneously.
Summary of the invention
In order to solve above-mentioned sulfuration not thoroughly, risk is relatively big, CS2 easily accumulates in the catalyst and after introducing technology gas very The easily technical problem of overtemperature, the present invention provides one to vulcanize thoroughly, risk is little, CS2 will not accumulate in the catalyst and lead After entering process gas, the change furnace catalyst low-pressure heater of overtemperature does not heats process gas vulcanizing equipment and vulcanization process thereof.
The present invention provide change furnace catalyst low-pressure heater heating process gas vulcanizing equipment, including steam heater, Catalyst, nitrogen aerator and process gas conversion pipeline, described catalyst is located at described steam heater, described nitrogen air blast Machine, described process gas conversion pipeline is connected with described steam heater, and described steam heater includes shell-side cylinder and is located at it In U-tube, catalyst rest area, nitrogen inlet, process gas entrance, nitrogen outlet, described U is located in described catalyst rest area Shape pipe one end, described nitrogen inlet, described process gas entrance and described nitrogen outlet are communicated in described U-tube.
In the change furnace catalyst low-pressure heater heating process gas vulcanizing equipment one preferred embodiment that the present invention provides In, described process gas conversion pipeline includes transformation system interlocking stop valve, and described work is located at by the chain stop valve of described transformation system Skill gas conversion pipeline.
The vulcanization process of the application change furnace catalyst low-pressure heater heating process gas vulcanizing equipment that the present invention provides, bag Include following steps:
Step one, catalyst tentatively vulcanize: be passed through circulating nitrogen gas outside described U-tube, then by described process gas entrance It is passed through the process gas containing hydrogen sulfide composition, controls hydrogen sulfide content in process gas, catalyst is tentatively vulcanized;
Step 2, the process gas content revulcanization that increases: be passed through a large amount of process gas by described process gas conversion pipeline and increase The hydrogen sulfide content added in nitrogen carries out degree of depth sulfuration to catalyst;
In step 3, increase process gas, hydrogen sulfide content carries out degree of depth sulfuration: by adding in gasification coal slurry preparation process Enter solid sulfate and increase the hydrogen sulfide content in process gas, catalyst is carried out degree of depth sulfuration.
The vulcanization process one of application change furnace catalyst low-pressure heater heating process gas vulcanizing equipment is provided in the present invention Planting in preferred embodiment, in described step one, the temperature range of preliminary sulfuration is 200 DEG C-300 DEG C.
The vulcanization process one of application change furnace catalyst low-pressure heater heating process gas vulcanizing equipment is provided in the present invention Plant in preferred embodiment, described step one is gradually increased process gas content by described process gas conversion pipeline.
The vulcanization process one of application change furnace catalyst low-pressure heater heating process gas vulcanizing equipment is provided in the present invention In kind of preferred embodiment, described step 2 increases the step of process gas content particularly as follows:
Step 2 one, nitrogen charge of suspending: suspend described nitrogen aerator, stop adding nitrogen to described steam heater Gas;
Step 2 two, the process gas that increases: gradually allocate process gas into by described process gas conversion pipeline;
Step 2 three, increase nitrogen charge: open described nitrogen aerator, be gradually added into nitrogen.
The vulcanization process one of application change furnace catalyst low-pressure heater heating process gas vulcanizing equipment is provided in the present invention In kind of preferred embodiment, described step 3 increases hydrogen sulfide content in process gas carry out degree of depth sulfuration step particularly as follows:
Step 3 one, nitrogen charge of suspending: suspend described nitrogen aerator, stop adding nitrogen to described steam heater Gas;
Step 3 two, the process gas that increases: gradually allocate process gas into by described process gas conversion pipeline.
The change furnace catalyst low-pressure heater heating process gas vulcanizing equipment of the present invention and vulcanization process thereof use gasification The process gas that stove produces carries out the method vulcanized, time saving and energy saving, and sulfuration is more thorough, and catalyst activity is extremely strong, and rate of change reaches 91.33%, initial vulcanization step change hearth layer temperature is the highest 370 DEG C, and inducing QI time-varying hearth layer temperature is the highest 470 DEG C, and basic holding puts down , there is not overheating problem in steady operation.
Accompanying drawing explanation
For the technical scheme being illustrated more clearly that in the embodiment of the present invention, in embodiment being described below required for make Accompanying drawing be briefly described, it should be apparent that, below describe in accompanying drawing be only some embodiments of the present invention, for From the point of view of those of ordinary skill in the art, on the premise of not paying creative work, it is also possible to obtain other according to these accompanying drawings Accompanying drawing, wherein:
Fig. 1 is change furnace catalyst low-pressure heater heating a kind of embodiment of process gas vulcanizing equipment that the present invention provides Structural representation;
Fig. 2 is the vulcanization process of the change furnace catalyst low-pressure heater heating process gas vulcanizing equipment shown in application drawing 1 The structural representation of a kind of embodiment;
Fig. 3 is the structural representation of a kind of embodiment of the step 2 of the vulcanization process shown in Fig. 2;
Fig. 4 is the structural representation of a kind of embodiment of the step 3 of the vulcanization process shown in Fig. 2.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete Describe, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments wholely.Based on Embodiment in the present invention, those of ordinary skill in the art obtained under not making creative work premise all other Embodiment, broadly falls into the scope of protection of the invention.
Seeing also Fig. 1 to Fig. 4, wherein Fig. 1 is the change furnace catalyst low-pressure heater heater that the present invention provides The structural representation of a kind of embodiment of skill gas vulcanizing equipment;Fig. 2 is that the change furnace catalyst low-pressure heater shown in application drawing 1 adds A kind of structural representation of the embodiment of the vulcanization process of heat technologic gas vulcanizing equipment;Fig. 3 is the step of the vulcanization process shown in Fig. 2 A kind of structural representation of the embodiment of rapid two;Fig. 4 is the structure of a kind of embodiment of the step 3 of the vulcanization process shown in Fig. 2 Schematic diagram.
Described change furnace catalyst low-pressure heater heating process gas vulcanizing equipment 1 includes steam heater 11, catalyst 12, nitrogen aerator 13, process gas conversion pipeline 14 and steam pipe line 15.Described steam heater is located at by described catalyst 12 11, described nitrogen aerator 13, described process gas conversion pipeline 14 is connected with described steam heater 11.Described process gas converts Pipeline 14 includes transformation system interlocking stop valve 141.Described process gas inverter tube is located at by the chain stop valve of described transformation system 141 Line 14, described steam pipe line 15 is connected with described steam heater 11.
Described steam heater 11 include shell-side cylinder 111 and the U-tube 112 being located therein, catalyst rest area 113, Nitrogen inlet 114, process gas entrance 115, nitrogen outlet 116.Described U-tube 112 1 is located in described catalyst rest area 113 End, described nitrogen inlet 114, described process gas entrance 115 and described nitrogen outlet 114 are communicated in described U-tube 112.
A kind of vulcanization process S1 applying change furnace catalyst low-pressure heater heating process gas vulcanizing equipment, its feature exists In, comprise the steps:
S11, catalyst tentatively vulcanize: be passed through circulating nitrogen gas outside described U-tube, then be passed through by described process gas entrance Containing the process gas of hydrogen sulfide composition, it is gradually increased process gas content specifically by described process gas conversion pipeline, controls work Hydrogen sulfide content in skill gas, tentatively vulcanizes catalyst, and the temperature range of preliminary sulfuration is 200 DEG C-300 DEG C;
S12, increase process gas content revulcanization: being passed through a large amount of process gas by described process gas conversion pipeline increases nitrogen Hydrogen sulfide content in gas carries out degree of depth sulfuration to catalyst;
Specifically include following steps:
S121, time-out nitrogen charge: suspend described nitrogen aerator, stop adding nitrogen to described steam heater;
S122, increase process gas: gradually allocate process gas into by described process gas conversion pipeline;
S123, increase nitrogen charge: open described nitrogen aerator, be gradually added into nitrogen.
In S13, increase process gas, hydrogen sulfide content carries out degree of depth sulfuration: solid by adding in gasification coal slurry preparation process Body sulfide increases the hydrogen sulfide content in process gas, and catalyst is carried out degree of depth sulfuration;
Specifically include following steps:
S131, time-out nitrogen charge: suspend described nitrogen aerator, stop adding nitrogen to described steam heater;
S132, increase process gas: gradually allocate process gas into by described process gas conversion pipeline.
Another preferred embodiment implementation process of the present invention is:
1, sulfuration first stage (heat up+a small amount of process gas):
First day 6:45 starts nitrogen aerator and heats up, and 19:45 mono-becomes furnace catalyst upper surface 260 DEG C, 234 DEG C of middle part, 221 DEG C, bottom, change furnace reaction bed temperature has been provided with conditions of vulcanization, and process gas initially enters change furnace, and 21:10 passes through Gasifying to conversion pipeline pressure-raising increase and allocate technique tolerance into, one becomes furnace catalyst upper surface 253.9 DEG C, 283.7 DEG C of middle part, bottom 299.2℃。
2, sulfuration second stage (heating nitrogen+process gas):
Second day 0:55, stops because of supercurrent due to nitrogen aerator, it is contemplated that cyclic nitrogen is large-minded, enters change furnace technique Tolerance is few, and nitrogen aerator supercurrent is agnogenio simultaneously, determines temporarily not start aerator, the most entirely opens supplementary nitrogen valve Entering a change stove, standard-sized sheet atmospheric valve to torch, nitrogen amount has 10260Nm3/h, pressure 0.05MPa, then opens new allotment of labor's skill gas pipeline Process gas gradually allocated into by hands valve, and slow raising is put governor pressure and risen to from 2.66kPa to 0.08MPa, observation one change furnace pressure difference 5.1kPa, continue to one become furnace catalyst sulfuration, 2:50, raising blowdown pressure is 0.2Mpa, nitrogen amount automatically reduce to 5700Nm3/h, pressure reduction is down to 3.39kpa, and due to process gas line pressure 0.8MPa, not quite, one becomes stove urges the change of process gas amount Agent variations in temperature is little.9:40, catalyst a manufacturer deems that allocates technique tolerance into very little, and bed temperature rise no longer changes, and again changes Become vulcanization process: start nitrogen aerator, open process gas main line flow process, slowly open XV-04101 bypass heating coil and enter to a change stove Mouthful main valve, qualified after slowly open a change stove entrance main valve and join process gas sulfuration.
3, sulfuration phase III (process gas boosts to 1.0MPa):
Second day 16:50, after all pressing unanimously, will open XV-before and after entering transformation system interlocking stop valve XV-04101 valve 04101, close its bypass, start gradually to open a change stove entrance main valve and increase technique tolerance, slowly exit circulating-heating nitrogen amount, 17:02, opens two changes, three change stoves import and export electrodynamic valves, heats up two changes, three change stoves, be promoted to by sulfide stress simultaneously 0.3MPa, 19:40, stop nitrogen aerator, all vulcanize by process gas, and sulfide stress is promoted to 0.4MPa, and the 3rd My god, 3:30, gradually transformation system pressure-raising is vulcanized, 6:00, change furnace all presses inducing QI, 7:30, and process gas all imports transformation series System, is vented to torch from PV-04282.8:50 sampling result is analyzed, and imports and exports sulfur content substantially suitable, and system pressure rises to behaviour Making pressure, warp and catalyst producer to confirm, sulfuration terminates.
Cure efficiency is analyzed:
1, beginning to warm to 7:30 sulfuration in the 3rd day from first day 6:45 qualified, process gas is vented after all entering conversion, uses Time 49 hours, plan 30 hours, beyond 19 hours.
2, to become hearth layer temperature the highest 370 DEG C for initial vulcanization step one, and during inducing QI, one to become hearth layer temperature the highest 470 DEG C, substantially Held stationary runs, and overheating problem does not occur.
3, the 4th day 10:00, when load is added to 100%, one becomes outlet of still CO content 3.76%, within 6 days one, becomes outlet of still CO Content 3.89%, it can be seen that, catalyst activity is extremely strong, and bed upper temp 365.1 DEG C, middle portion temperature 434.5 DEG C, bottom Temperature 435.6 DEG C, inlet temperature 279.8 DEG C, outlet temperature 432 DEG C, rate of change reaches 91.33%.
The change furnace catalyst low-pressure heater heating process gas vulcanizing equipment of the present invention and vulcanization process 1 thereof have as follows Beneficial effect:
The change furnace catalyst low-pressure heater heating process gas vulcanizing equipment of the present invention and vulcanization process thereof use gasification The process gas that stove produces carries out the method vulcanized, time saving and energy saving, and sulfuration is more thorough, and catalyst activity is extremely strong, and rate of change reaches 91.33%, initial vulcanization step change hearth layer temperature is the highest 370 DEG C, and inducing QI time-varying hearth layer temperature is the highest 470 DEG C, and basic holding puts down , there is not overheating problem in steady operation.
The foregoing is only embodiments of the invention, not thereby limit the scope of the claims of the present invention, every utilize this Equivalent structure or equivalence flow process that bright description and accompanying drawing content are made convert, or are directly or indirectly used in other relevant skill Art field, is the most in like manner included in the scope of patent protection of the present invention.

Claims (7)

1. change furnace catalyst low-pressure heater heating process gas vulcanizing equipment, it is characterised in that include steam heater, Catalyst, nitrogen aerator and process gas conversion pipeline, described catalyst is located at described steam heater, described nitrogen air blast Machine, described process gas conversion pipeline is connected with described steam heater, and described steam heater includes shell-side cylinder and is located at it In U-tube, catalyst rest area, nitrogen inlet, process gas entrance, nitrogen outlet, described U is located in described catalyst rest area Shape pipe one end, described nitrogen inlet, described process gas entrance and described nitrogen outlet are communicated in described U-tube.
Change furnace catalyst low-pressure heater the most according to claim 1 heating process gas vulcanizing equipment, it is characterised in that Described process gas conversion pipeline includes transformation system interlocking stop valve, and described process gas is located at by the chain stop valve of described transformation system Conversion pipeline.
3. any one the change furnace catalyst low-pressure heater heating process gas sulfur that one kind is applied described in claim 1 to 2 The vulcanization process of change equipment, it is characterised in that comprise the steps:
Step one, catalyst tentatively vulcanize: be passed through circulating nitrogen gas outside described U-tube, then be passed through by described process gas entrance Containing the process gas of hydrogen sulfide composition, control hydrogen sulfide content in process gas, catalyst is tentatively vulcanized;
Step 2, the process gas content revulcanization that increases: being passed through a large amount of process gas by described process gas conversion pipeline increases nitrogen Hydrogen sulfide content in gas carries out degree of depth sulfuration to catalyst;
In step 3, increase process gas, hydrogen sulfide content carries out degree of depth sulfuration: solid by adding in gasification coal slurry preparation process Body sulfide increases the hydrogen sulfide content in process gas, and catalyst is carried out degree of depth sulfuration.
Vulcanization process the most according to claim 3, it is characterised in that in described step one, the temperature range of preliminary sulfuration is 200℃-300℃。
Vulcanization process the most according to claim 3, it is characterised in that by described process gas inverter tube in described step one Line is gradually increased process gas content.
Vulcanization process the most according to claim 3, it is characterised in that increase the step of process gas content in described step 2 Particularly as follows:
Step 2 one, nitrogen charge of suspending: suspend described nitrogen aerator, stop adding nitrogen to described steam heater;
Step 2 two, the process gas that increases: gradually allocate process gas into by described process gas conversion pipeline;
Step 2 three, increase nitrogen charge: open described nitrogen aerator, be gradually added into nitrogen.
Vulcanization process the most according to claim 3, it is characterised in that increase hydrogen sulfide in process gas in described step 3 and contain Amount carry out degree of depth sulfuration step particularly as follows:
Step 3 one, nitrogen charge of suspending: suspend described nitrogen aerator, stop adding nitrogen to described steam heater;
Step 3 two, the process gas that increases: gradually allocate process gas into by described process gas conversion pipeline.
CN201610766651.0A 2016-08-30 2016-08-30 Change furnace catalyst low-pressure heater heating process gas vulcanizing equipment and vulcanization process thereof Pending CN106268975A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1475140A1 (en) * 2003-05-07 2004-11-10 Kocat Inc. Catalyst and process for nitrogen oxides reduction in combustion exhaust gas
CN103657741A (en) * 2012-09-19 2014-03-26 中国石油化工股份有限公司 Method for circularly and rapidly pre-vulcanizing sulfur tolerant shift catalyst and carrying out segmental pre-vulcanizing by utilizing sulfur tolerant shift catalyst
CN103657740A (en) * 2012-09-19 2014-03-26 中国石油化工股份有限公司 Step-by-step sulfuration method of sulfur tolerant shift catalyst

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1475140A1 (en) * 2003-05-07 2004-11-10 Kocat Inc. Catalyst and process for nitrogen oxides reduction in combustion exhaust gas
CN103657741A (en) * 2012-09-19 2014-03-26 中国石油化工股份有限公司 Method for circularly and rapidly pre-vulcanizing sulfur tolerant shift catalyst and carrying out segmental pre-vulcanizing by utilizing sulfur tolerant shift catalyst
CN103657740A (en) * 2012-09-19 2014-03-26 中国石油化工股份有限公司 Step-by-step sulfuration method of sulfur tolerant shift catalyst

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