CN106423160B - The guard method of catalyst when coal-ethylene glycol dehydrogenation purification process stops in emergency - Google Patents

The guard method of catalyst when coal-ethylene glycol dehydrogenation purification process stops in emergency Download PDF

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CN106423160B
CN106423160B CN201610848508.6A CN201610848508A CN106423160B CN 106423160 B CN106423160 B CN 106423160B CN 201610848508 A CN201610848508 A CN 201610848508A CN 106423160 B CN106423160 B CN 106423160B
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catalyst
reactor
gas
coal
ethylene glycol
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CN106423160A (en
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姚元根
周张锋
乔路阳
宗珊珊
崔国静
吴娟
潘鹏斌
林凌
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Fujian Institute of Research on the Structure of Matter of CAS
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    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/56—Platinum group metals
    • B01J23/63—Platinum group metals with rare earths or actinides
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • 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
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Catalysts (AREA)

Abstract

The guard method of catalyst, the catalyst are PdO CeO when stopping in emergency the invention discloses a kind of coal-ethylene glycol dehydrogenation purification process2/Al2O3Catalyst.The guard method is carried out in coal-ethylene glycol dehydrogenation cleaning catalyst reaction unit.When encountering emergency case needs emergency stop protection, it is first turned off O2Air inlet gas circuit; it prevents from continuing that exothermic oxidation reaction occurs in dehydrogenation purification reactor; stop carrying out the pre-heat treatment to reaction mass; the reaction mass of room temperature is passed through to move heat; it is passed through low temperature again and moves thermal medium to realize fast cooling; the air speed for being passed through inert gas simultaneously, continuously decreasing CO unstripped gas, the blanketing with inert gas after temperature reduction.The catalyst handled with the guard method is suitable with the catalyst activity before emergency case.Compared with prior art, its main feature is that easy to operate, material consumption is few, and low energy consumption, and the operation carried out will not have an impact the other technique units of coal-ethylene glycol, be particularly suitable for commercial plant.

Description

The guard method of catalyst when coal-ethylene glycol dehydrogenation purification process stops in emergency
Technical field
The present invention relates to a kind of guard methods of catalyst, and in particular to a kind of coal-ethylene glycol technology dehydrogenation purifying and catalyzing Agent in driving process an emergency situation is encountered parking when guard method.
Background technology
The filling of catalyst and unloading process are cumbersome on industrialized unit, especially calandria type fixed bed reactor Catalyst is in filling, it is necessary to assure and the loadings of every tubulation are consistent, and test pressure drop is also needed after each tubulation loading catalyst, Generally to ensure that pressure drop no more than 5% is not in just reaction mass short circuit phenomenon.Therefore, Catalyst packing is good under normal circumstances It no longer unloads afterwards, unless because catalyst inactivation needs replacing catalyst and just recharged.
However, industrialized unit can inevitably be influenced by some external factors and have no alternative but stop in emergency at runtime, Mainly there are following a few class situations：
(1) failure of the mating compressor of reactor, heat exchanger, pipeline, valve member；
(2) technology of some process routes length, the wherein device of the front and back workshop section of some reaction break down, such as coal system Ethylene glycol technology has 6 reaction members, the failure of any one reaction member that can all influence other several reaction members just Often operation；
(3) technological transformation.
When there is above-mentioned emergency case, it need to stop in emergency reactor with guard catalyst.Processing stop in emergency not When the damage that can cause unrepairable to the catalyst in reactor, lead to catalyst activity reduction even complete deactivation.Currently, The most important guard method of catalyst is generally by the protective device that one auxiliary of some protective agents or addition is added or passes through Inert gas is passed through to realize.
Patent CN2013201956390 reports a kind of catalyst protection device, which is connected with reactor, including upper There is the inert gas holding vessel of exhaust outlet at end, and ftercompction pneumatic control valve is provided between reactor and inert gas holding vessel, mends Pressure pneumatic control valve one end is connect with the exhaust outlet of inert gas holding vessel, the gas supplementing opening connection of the other end and reactor.The hair Bright technology needs additional increase set of device, increases cost of investment.
Patent CN201210587005X reports a kind of protective agent of catalyst for partially oxidizing conversion, the protective agent quality Percentage component includes for nickel oxide 5~6%, α-Al2O378~85%, silica 4~6%, magnesia 1~5%, dioxy Change manganese 1~5%；The protective agent is applied to be combined as in oil refinery dry gas, natural gas or the light oil type and others for having combustion space The partial oxidation reforming technique that raw material carries out.But protectant addition may not only cause some side reactions, but also increase The volume of fixed bed reactors, increases cost of investment.
Patent CN2011100027301 reports a kind of control system preventing the catalyst breakage in cutoff event, packet Temperature determination module and catalyst protection module are included, the resistance of heating element of the temperature determination module based on oxygen sensor is come really Surely the temperature being vented.When the temperature of exhaust is more than threshold temperature, the operating parameter that catalyst protection module adjusts engine comes Reduce the temperature of exhaust, temperature of the threshold temperature based on the catalyst in damage exhaust system.But the addition of control system carries The high requirement to control, and increase cost of investment.
Therefore, in order to overcome existing technological deficiency, a kind of inexpensive, guard method easy to operate is provided, to industry Disguising the reactor processing that an emergency situation is encountered in driving process set is particularly important.
Invention content
The protection side of catalyst when stopping in emergency the object of the present invention is to provide a kind of coal-ethylene glycol dehydrogenation purifier Method, the present invention reduce steam inlet amount to reduce temperature of reactor, improve the reaction of room temperature by emergency cut-off oxidizing gas The processing method that the internal circulating load of unstripped gas (or inert gas) is combined can play very coal-ethylene glycol dehydrogenation cleaning catalyst Good protective effect.
The guard method of catalyst, that is, exist when a kind of coal-ethylene glycol dehydrogenation purifier of the present invention stops in emergency In ethylene glycol dehydrogenation purification reactor, when encountering emergency case needs emergency stop protection, it is first turned off O2Air inlet gas circuit, prevents Continue that exothermic oxidation reaction occurs in dehydrogenation purification reactor, stops carrying out the pre-heat treatment to reaction mass, be passed through the anti-of room temperature It answers material to be conducive to move heat, then reduces steam inlet amount to realize fast cooling, while being passed through inert gas, continuously decreasing CO originals The air speed for expecting gas, the blanketing with inert gas after temperature reduction.The catalyst handled with the guard method occurs with emergency case Preceding catalyst activity is suitable, can play the role of guard catalyst well, and driving rear catalyst still can be again A small amount of H in CO unstripped gas2It is removed to 100ppm or less.
Catalyst used in coal-ethylene glycol dehydrogenation purification process is PdO-CeO2/Al2O3, wherein Pd mass percentages It is 0.05-2.0%, preferable content is that 0.1-1.0%, Ce mass percentages are 0.1-5%, and preferable content is 0.2- 2.0%, the ball-aluminium oxide of a diameter of 2-3mm of alumina support used, crystal form is γ-Al2O3。
Fig. 1 is coal-ethylene glycol dehydrogenation cleaning catalyst reaction member, wherein 1 be feed gas containing carbon monoxide body entrance, 2 It is inert gas entrance for oxygen intake, 3,4 be gas compressor, and 5 be gas preheater before reactor, and 6 be gas before reactor Body preheater intake valve, 7 be gas preheater air outlet valve before reactor, and 8 be gas preheater gas short valve before reactor, 9 For dehydrogenation purification reactor, 10 be steam into dehydrogenation purification reactor entrance, and 11 go out the outlet of dehydrogenation purification reactor for steam, 12 It is liquid water storage tank for gas-liquid separator, 13,14 be drain, and 15 be mole sieve drier, and 16 be triple valve, and 17 be an oxidation Enter reaction pipeline in next step after carbon raw material qi exhaustion hydrogen purification, 18 be on-line chromatograph detector.
The guard method of coal-ethylene glycol dehydrogenation purifier catalyst when stopping in emergency of the present invention, it is specific to walk It is rapid as follows：
A. after an emergency situation is encountered O is closed in 30 minutes2Intake valve；Oxidizing gas O in quick cut-out system2, allow The oxidation reaction being happened in reactor stops, and is conducive to reactor cooling；
B. the gas preheater short valve before reactor is opened, closes gas preheater into and out of air valve；It allows after compressor Reaction gas before entering the reactor without preheating, the shifting heat that reactor is conducive to reactor is entered with lower temperature.
C. the steam inlet flow of reactor, the steam off intake valve in 1-3h, the temperature of reactor are continuously decreased Control is at 40-100 DEG C.Step C and step B are carried out at the same time.
D. inert gas intake valve is opened, air speed is controlled in 500-5000h-1；The inert gas is N2。
E. the flow of CO unstripped gas is gradually decreased, until completely closing；The step is after the operation for completing step A in 1-6h It completes
F. with N2CO unstrpped gases in metathesis reactor adjust emptying amount 1-20%, until following by drain CO raw material Gas contents in ring gas are less than 5%, O2Content is less than 0.5%；Gas content in circulating air passes through online gas phase color Spectrometer measures.
G. when temperature is reduced to 50 DEG C or less, the seal protection under circulating air atmosphere；Complete protection operation.
When device meets driving condition again, operation of driving again.
The present invention is that the best urgent protection processing scheme come is summed up on the basis of a series of contrast experiment, and existing Technology is compared, its main feature is that easy to operate, material consumption is few, and low energy consumption, emergency measure coal-ethylene glycol dehydrogenation reactor unit into Row, the operation carried out will not have an impact the other technique units of coal-ethylene glycol, the catalyst after protection operation and operation Preceding activity quite, is particularly suitable for commercial plant.
Description of the drawings
Fig. 1 is coal-ethylene glycol dehydrogenation purifier reaction member schematic diagram, wherein 1 enters for feed gas containing carbon monoxide body Mouthful, 2 be oxygen intake, and 3 be inert gas entrance, and 4 be gas compressor, and 5 be gas preheater before reactor, and 6 be reactor Preceding gas preheater intake valve, 7 be gas preheater air outlet valve before reactor, and 8 be gas preheater gas short circuit before reactor Valve, 9 be dehydrogenation purification reactor, and 10 be steam inlet, and 11 be steam (vapor) outlet, and 12 be gas-liquid separator, and 13 be liquid water storage tank, 14 be drain, and 15 be mole sieve drier, and 16 be triple valve, and 17 be to enter in next step after feed gas containing carbon monoxide dehydrogenation purifies Pipeline is reacted, 18 be on-line chromatograph detector.
Specific implementation mode
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Prepare PdO-CeO2/Al2O3Catalyst is that 0.8%, Ce mass percentages are according to Pd mass percentages 0.5%, the dosage of required palladium nitrate, cerous nitrate is calculated according to the mass content of the quality of alumina support and Pd, Ce, is pressed Palladium nitrate and cerous nitrate are dissolved in the dilute nitric acid solution that mass concentration is 1% by the dosage prepares dipping solution, Pd in solution Mass percentage be 0.8%, Ce mass percentage be 0.5%, then be thereto added isometric with dipping solution Spherical alumina support, the spherical alumina support are the γ-Al of a diameter of 2-3mm2O3, filtered out after impregnating 8h, in 150 DEG C of bakings Required PdO-CeO is made then at 450 DEG C of roasting 16h in dry 8h2/Al2O3Catalyst.
Embodiment 1
In device shown in Fig. 1, it is net that coal-ethylene glycol dehydrogenation is carried out on 100ml mold trial devices using the method for the present invention Changing catalyst, promptly protection is handled.
A. by PdO-CeO2/Al2O3Catalyst packing enters the dehydrogenation purification fixed bed reactors 9 of a diameter of 100ml scales, It is passed through N through 32Purge 20min, the temperature of preheater 5 is controlled at 125 DEG C, and the temperature of 135 DEG C of steam reactor 9 is passed through from 10 Degree is raised to 130 DEG C from room temperature, closes N2, it is passed through CO unstripped gas and the O of metering2It is reacted, hydrogen content is in CO unstripped gas 1.0%；VH2：VO2=1:2, pressure 0.3MPa, total air speed are 2000h-1, the gas after reaction is in 18 progress on-line chromatograph inspections It surveys, successive reaction 50h, the H after reaction2Content is always held at 10-20ppm.Assuming that subsequent carbonylation synthesis unit parking, needs Stop the supply of CO unstripped gas, coal-ethylene glycol dehydrogenation clean unit is carried out to simulate experiment of stopping in emergency.2 are closed in 10 minutes O2Intake valve.
B. open gas preheater short valve 8 before reactor, close gas preheater before reactor into and out of 6 He of air valve 7。
C. 10 steam inlet flows are continuously decreased, steam off intake valve after 2h controls the temperature of reactor 9 60 ℃。
D. the CO raw gas flows for gradually decreasing 1, from air speed 2000h in 1h-1It is reduced to 1000h-1It is passed through afterwards from 103 N2, N2Air speed control in 2000h-1, open drain and close CO unstripped gas intake valves after 14,30 minutes, the control of emptying amount exists 15%, until the CO raw material Gas contents in circulating air are less than 5%, O2Content is less than 0.5%.
E. when the temperature of reactor 9 is reduced to 50 DEG C, each terminal valve of reactor, seal protection are closed.
F. after G completes 100h, close gas preheater short valve 8 before reactor, open preheater into and out of air valve 6 With 1, it is passed through reaction gas with reference to the reaction step of A and is reacted again, the gas after reaction carries out on-line chromatograph detections 18, H2Content is 18ppm, suitable with the value in step A, it was demonstrated that this guard method is effective.
Embodiment 2
In device shown in Fig. 1, coal second is carried out on 1000 tons/year of ethylene glycol pilot-plants using the method for the present invention Promptly protection is handled two alcohol dehydrogenase cleaning catalysts.
A. by PdO-CeO2/Al2O3Catalyst packing enters the dehydrogenation purification fixed-bed column reactor 9 of a diameter of 700mm, It is passed through N through 32120min is purged, be passed through 135 DEG C of steam from 10 is raised to 130 DEG C the temperature of reactor 109, closes N2, it is passed through CO The O of unstripped gas and metering2It is reacted, hydrogen content is 1.0% in CO unstripped gas；VH2：VO2=1:2, pressure 0.3MPa, it is total empty Speed is 2000h-1, the gas after reaction is in 18 progress on-line chromatograph detections, successive reaction 100h, the H after reaction2Content is protected always It holds in 20-30ppm.
B. assume subsequent carbonylation synthesis unit parking, the supply of CO unstripped gas need to be stopped, coal-ethylene glycol dehydrogenation is purified Unit carries out simulating experiment of stopping in emergency.
C. 2 O is closed in 20 minutes2Intake valve.
D. open gas preheater short valve 8 before reactor, close gas preheater before reactor into and out of 6 He of air valve 7。
E. 10 steam inlet flows are continuously decreased, steam off intake valve after 2h controls the temperature of reactor 9 65 ℃。
F. the CO raw gas flows for gradually decreasing 1, from air speed 2000h in 3h-1It is reduced to 1000h-1Afterwards N is passed through from 32, N2Air speed control in 2000h-1, drain 14 is opened, CO unstripped gas intake valves are closed after 2h, emptying amount is controlled 15%, directly It is less than 5%, O to the CO raw material Gas contents in circulating air2Content is less than 0.5%.
G. when the temperature of reactor 9 is reduced to 50 DEG C, each terminal valve of reactor, seal protection are closed.
H. after G completes 100h, close gas preheater short valve 8 before reactor, open preheater into and out of air valve 6 With 7, it is passed through reaction gas with reference to the reaction step of A and is reacted again, the gas after reaction carries out on-line chromatograph detections 18, H2Content is 28ppm.Prove that this guard method is after enlarged experiment or effective.

Claims (2)

  1. The guard method of catalyst when 1. a kind of coal-ethylene glycol dehydrogenation purification process stops in emergency, this method is in coal-ethylene glycol It carries out, is as follows on dehydrogenation cleaning catalyst reaction unit：
    A. after an emergency situation is encountered O is closed in 30 minutes2Intake valve；Oxidizing gas O in quick cut-out system2, allow generation Oxidation reaction in reactor stops, and is conducive to reactor cooling；
    B. the gas preheater short valve before reactor is opened, closes gas preheater into and out of air valve；It allows anti-after compressor It answers gas before entering the reactor without preheating, the shifting heat that reactor is conducive to reactor is entered with lower temperature；
    C. the steam inlet flow of reactor is continuously decreased, the steam off intake valve in 1-3h controls the temperature of reactor At 40-100 DEG C；Step C and step B are carried out at the same time；
    D. inert gas intake valve is opened, air speed is controlled in 500-5000h-1；The inert gas is N2；
    E. the flow of CO unstripped gas is gradually decreased, until completely closing；The step is complete in 1-6h after the operation for completing step A At；
    F. with N2CO unstrpped gases in metathesis reactor adjust emptying amount 1-20%, until in circulating air by drain CO raw material Gas contents be less than 5%, O2Content is less than 0.5%；Gas content in circulating air is surveyed by on-line gas chromatography It is fixed；
    G. when temperature is reduced to 50 DEG C or less, the seal protection under circulating air atmosphere；Complete protection operation.
  2. The guard method of catalyst when 2. coal-ethylene glycol dehydrogenation purification process according to claim 1 stops in emergency, It is characterized in that the catalyst is PdO-CeO2/Al2O3, wherein Pd mass percentages are that 0.1-1.0%, Ce mass percentages contain Amount is 0.2-2.0%, and carrier used is the spherical gamma-Al of a diameter of 2-3mm2O3。
CN201610848508.6A 2016-09-26 2016-09-26 The guard method of catalyst when coal-ethylene glycol dehydrogenation purification process stops in emergency Active CN106423160B (en)

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Publication number Priority date Publication date Assignee Title
CN112129852B (en) * 2020-08-31 2021-08-10 中国科学院福建物质结构研究所 Reaction gas cyclic utilization and controllable CO dehydrogenation of atmosphere purifies catalyst evaluation device

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