CN105400553B - The method for changing one-level hydrogenation catalyst in coke-stove gas methanol device - Google Patents

The method for changing one-level hydrogenation catalyst in coke-stove gas methanol device Download PDF

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CN105400553B
CN105400553B CN201510748134.6A CN201510748134A CN105400553B CN 105400553 B CN105400553 B CN 105400553B CN 201510748134 A CN201510748134 A CN 201510748134A CN 105400553 B CN105400553 B CN 105400553B
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catalyst
level
coke
hydrogenation catalyst
hydrogenation
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CN105400553A (en
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孟祥辉
袁守敬
曹继温
刘慧�
袁金柱
吴春松
闪俊杰
刘艳飞
孙春凯
王磊
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TANGSHAN ZHONGRUN COAL CHEMICAL INDUSTRY Co Ltd
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TANGSHAN ZHONGRUN COAL CHEMICAL INDUSTRY Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
    • C10K1/00—Purifying combustible gases containing carbon monoxide
    • C10K1/32—Purifying combustible gases containing carbon monoxide with selectively adsorptive solids, e.g. active carbon
    • 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
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/889—Manganese, technetium or rhenium
    • B01J23/8892—Manganese
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Materials Engineering (AREA)
  • Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a kind of method for changing one-level hydrogenation catalyst in coke-stove gas methanol device, it uses following method and steps：（1）By each filter stop successively and by filler replacement be wood activated charcoal oil absorbent；（2）Groove parking will be hydrogenated with advance, change the catalyst for pre-hydrogenation in it；（3）One-level is hydrogenated with to first after groove middle temperature zinc oxide bath parking, its catalyst change ferrimanganic desulphurization catalyst loaded；（4）One-level is hydrogenated with to second after groove middle temperature zinc oxide bath parking, change the outfit iron molybdenum hydrogenation catalyst on its upper strata；（5）One-level is hydrogenated with and stopped, system is incorporated to after more one-level hydrogenation catalyst and is vulcanized online.This method passes through more catalyst changeout, it is ensured that the conversion ratio of organic sulfur, temporarily substitutes the effect of one-level hydrogenation, fine de-sulfur is exported sulfur content and is less than 0.1PPM, so as to be allowed to not stop to change one-level hydrogenation catalyst in the case of production.

Description

The method for changing one-level hydrogenation catalyst in coke-stove gas methanol device
Technical field
The present invention relates to a kind of fine desulfurizing technology process suitable for coal chemical industry enterprises coke-stove gas methanol, especially one Plant the method for changing one-level hydrogenation catalyst in coke-stove gas methanol device.
Background technology
Coal chemical industry enterprises are raw material using coke-stove gas, by desulfurization, are converted, synthesis, and the process such as rectifying prepares methanol.Figure Shown in 1, in fine de-sulfur workshop section, the oven gas from oven gas compression section is de- by oil eliminator, filter A and filter B Tar removing, then after pre- desulfurizer removing partial vulcanization thing, go the first preheater of oven gas of conversion section to be preheated.Fig. 2 Shown, the oven gas after preheating is returned in the pre- hydrogenation groove and one-level hydrogenation groove of fine de-sulfur device, the big portion of organic sulfur in gas Divide and be converted into inorganic sulfur (H2S)；Then by middle temperature zinc oxide bath A, middle temperature zinc oxide bath B and middle temperature zinc oxide bath C removings H2S； Gas enters secondary hydrogenation groove afterwards, is inorganic sulfur by remaining organic sulfur conversion, zinc oxide bath A and zinc oxide bath are finally passed through again The further desulfurization of B, makes total sulfur content≤0.1ppm of gas, delivers to conversion section.Above-mentioned filter A, filter B and pre- de- Efficient oil absorbent is loaded among sulphur groove, is hydrogenated with advance among groove, one-level are hydrogenated with groove and secondary hydrogenation groove and all loads iron molybdenum hydrogenation catalyst Agent.
The one-level hydrogenation catalyst loaded in one-level hydrogenation groove is that the crucial production of methanol process fine de-sulfur workshop section will Element, by one-level hydrogenation catalyst by the organic sulfur conversion in coke-stove gas be inorganic sulfur, zinc oxide, iron oxide desulphurization catalyst Desulphurization reaction could be carried out.However, traditional one-level hydrogenation catalyst Replacing Scheme needs the ability in the case where device stops Carry out, otherwise the organic sulfur of fine de-sulfur workshop section outlet can exceed technic index, and irreversible murder by poisoning is caused to methanol synthesis catalyst. One-level hydrogenation catalyst is changed to add by cooling, replacing, loading and unloading, heating up, vulcanizing, put sulphur, be incorporated to 6 steps of system The device driving and parking time, change an one-level hydrogenation catalyst at least need 10 day time, exist down time it is long, reduction dress Put the weak points such as the utilization of capacity, influence methanol output.
The content of the invention
Add the technical problem to be solved in the present invention is to provide one-level in a kind of onstream replacement coke-stove gas methanol device The method of hydrogen catalyst.
In order to solve the above technical problems, the present invention uses following method and steps：
(1) by each filter stop successively and by filler replacement be wood activated charcoal oil absorbent；
(2) groove parking will be hydrogenated with advance, change the catalyst for pre-hydrogenation in it；
(3) one-level is hydrogenated with to first middle temperature zinc oxide bath after groove to stop, its catalyst change ferrimanganic desulfurization loaded Catalyst；
(4) one-level is hydrogenated with to second middle temperature zinc oxide bath after groove to stop, change the outfit iron molybdenum hydrogenation catalyst on its upper strata；
(5) one-level is hydrogenated with and stopped, be incorporated to system after more one-level hydrogenation catalyst and vulcanized online.
In step (2) of the present invention, the loadings standard of catalyst for pre-hydrogenation is, catalyst space velocities 5000~ 6000NM3/m3·h。
In step (3) of the present invention, the loadings standard of ferrimanganic desulphurization catalyst is, catalyst space velocities 500~ 700NM3/m3·h。
In step (4) of the present invention, the loadings standard for the hydrogenation catalyst that changes the outfit is, catalyst space velocities 5000~ 6000NM3/m3·h。
In step (1) of the present invention, wood activated charcoal oil absorbent is HT-203 activated carbon oil absorbents.
Before step (1) of the present invention, by adjusting the doctor solution internal circulating load of the wet desulfurization workshop section in upstream, improve workshop section and go out Mouth hydrogen sulfide in coke oven content.Workshop section outlet hydrogen sulfide in coke oven content is improved to 90~110mg/NM3。
It is using the beneficial effect produced by above-mentioned technical proposal：1st, the wood activated charcoal newly changed, especially HT- 203 activated carbon oil absorbents are all higher than the efficient clay oil absorbents of original TX-1 in oil capacity and porosity, can effectively protect hydrogenation Catalyst, extends the hydrogenation catalyst life-span.2nd, the new organic sulfur conversion rate for changing ferrimanganic desulphurization catalyst, can be effective up to 80% Part substitutes the effect of one-level hydrogenation catalyst, while hydrogen sulfide can be absorbed, reduces the pressure of zinc oxide B and C depriving hydrogen sulphide, Ensure that fine de-sulfur outlet sulfur content meets index.The present invention passes through more catalyst changeout, it is ensured that the conversion ratio of organic sulfur, temporarily substitutes The effect of one-level hydrogenation, makes fine de-sulfur export sulfur content and is less than 0.1PPM, so as to be allowed to not stop to change one in the case of production Level hydrogenation catalyst；Through calculating, apply the present invention to 200,000 tons/year of coke-stove gas methanol system, dress can be effectively improved Put the utilization of capacity, year can about 3800 tons of increase yield of methanol, annual benefit is about up to 9,500,000 yuan.The present invention is by adjusting the wet desulfurization in upstream The doctor solution internal circulating load of workshop section, makes workshop section export hydrogen sulfide in coke oven content and improves to 90~110mg/NM3, to new replacing Catalyst for pre-hydrogenation vulcanized online, it is ensured that the good organic sulfur conversion efficiency of catalyst.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 and 2 is the process equipment schematic diagram of the present invention.
Embodiment
Shown in Fig. 1, Fig. 2, the concrete technology of the method for one-level hydrogenation catalyst in this replacing coke-stove gas methanol device Step is：(1) the efficient oil absorbents of TX-1 loaded filter A, filter B originally are replaced by wood activated charcoal, preferably HT- 203 activated carbon oil absorbents；To be changed successively during replacing, i.e. first shut-down filter A (filter B), change above-mentioned oil absorbent, reach the standard grade Stop work again afterwards filter B (filter A), change described oil absorbent.(2) catalyst for pre-hydrogenation in pre- hydrogenation groove is changed, is led to Overregulating the wet desulfurization workshop section doctor solution internal circulating load in upstream makes hydrogen sulfide outlet content in outlet be 90~110mg/NM3, preferably 100mg/NM3, the catalyst for pre-hydrogenation newly changed is vulcanized online, it is ensured that the good organic sulfur conversion efficiency of catalyst； The loadings standard of catalyst for pre-hydrogenation：5000~6000NM of catalyst space velocities3/m3·h；With single Jiao for covering 100,000 tons/year of annual output Exemplified by producer gas methanol device, catalyst for pre-hydrogenation amount of fill is 5~6m3.(3) one-level is hydrogenated with first middle temperature after groove Zinc oxide bath-middle temperature zinc oxide bath A internal oxidition zinc desulphurization catalysts are replaced by ferrimanganic desulphurization catalyst, are urged using ferrimanganic desulfurization The organic sulfur conversion function that agent possesses；Iron-manganese desulfurizer can absorb hydrogen sulfide simultaneously, reduce middle temperature zinc oxide bath B with The pressure of warm zinc oxide bath C depriving hydrogen sulphides, it is ensured that fine de-sulfur outlet sulfur content meets index；The loadings of ferrimanganic desulphurization catalyst Standard：500~700NM of catalyst space velocities3/m3·h；Exemplified by singly covering and produce 100000 tons/year of coke-stove gas methanol device per year, Ferrimanganic desulphurization catalyst amount of fill is 50~70m3.(4) iron molybdenum hydrogenation catalyst is loaded on middle temperature zinc oxide bath B top；Plus The loadings standard of hydrogen catalyst：5000~6000NM of catalyst space velocities3/m3·h；With single coke-oven coal for covering 100,000 tons/year of annual output , will the 52m that originally loaded of middle temperature zinc oxide bath B exemplified by gas methanol device3Zinc oxide catalytic, be changed to lower floor 46~ 47m3Zinc oxide catalytic is motionless, 5~6m of upper strata3Zinc oxide catalytic is adapted as 5~6m3Iron molybdenum hydrogenation catalyst；Further Organic sulfur conversion rate is improved, the groove is possessed the dual-use function that conversion absorbs organic sulfur.(5) by adjusting desulfurization workshop section upstream Wet desulfurization workshop section doctor solution internal circulating load, Shi Shi desulfurization workshop section exit hydrogen sulfide content is 90~110mg/NM3, to new clothes one-level Hydrogenation catalyst is vulcanized online.Desulfurization workshop section upstream refers to wet desulfurization workshop section, using sodium carbonate wet desulphurization, passes through Doctor solution (mainly based on sodium carbonate and PDS catalyst solutions) is inversely contacted, absorbing and removing vulcanization therein with coke-stove gas Hydrogen, hydrogen sulfide in coke oven content≤20mg/NM of the normal wet desulfurization workshop section outlet of production requirement3；This method is in order to under Trip fine de-sulfur workshop section newly changes hydrogenation catalyst and vulcanized online, reduces desulfurization liquid measure, workshop section is exported sulphur in coke oven gas Change hydrogen content raising and be maintained at 90~110mg/NM3, preferably 100mg/NM3。
Embodiment：Exemplified by using this method in the coke-stove gas methanol system at 200,000 tons/year, pre- hydrogenation groove filling Measure as 5m3, coal gas amount is 30000NM3/ h, therefore air speed is 6000NM3/(h·m3), hydrogenation catalyst is organic under this air speed Sulphur conversion ratio is 60% or so.The loadings of the organic sulfur of ferrimanganic desulphurization catalyst are 52m3, organic sulfur conversion rate is 80%.Oxygen Change zinc groove A tops and 5m is housed3, therefore organic sulfur conversion rate is similarly 60%.Secondary hydrogenation groove loadings are 17m3, coal gas amount is 30000NM3/ h, therefore air speed is 1768NM3/(h·m3), the organic sulfur conversion rate of hydrogenation catalyst is 90% under this air speed.Essence is de- Organic sulfur content is about 150mg/m in sulphur entrance coal gas3, after one-level hydrogenation catalyst is cut out, utilize catalyst for pre-hydrogenation, iron Iron molybdenum hydrogenation catalyst and secondary hydrogenation catalyst removal organic sulfur are loaded on manganese desulphurization catalyst, middle temperature zinc oxide bath B, therefore Export organic sulfur content=150 × (1-0.6) × (1-0.8) × (1-0.6) × (1-0.9)=0.48mg/m3＜ 0.1PPM, therefore Outlet organic sulfur meets index.By above-mentioned calculating formula, secondary hydrogenation can convert 4.32mg/m3Organic sulfur, equivalent to every Hour release 0.0018g hydrogen sulfide, discharges hydrogen sulfide 0.4g hydrogen sulfide in 10 days, latter two zinc oxide bath of secondary hydrogenation is filled altogether altogether 20m3Zinc oxide desulfurizer, zinc oxide Sulfur capacity is about 30%, therefore hydrogen sulfide will be completely absorbed.
Above-mentioned raw materials：Activated carbon oil absorbent is HT-203, the production of Shandong Zibo Hai Chuan Fine Chemical Co., Ltd；Ferrimanganic takes off Sulfur catalyst is W704, Wuhan Kelin Fine Chemical Co., Ltd.'s production；Iron molybdenum hydrogenation catalyst is T202C, Beijing trimerization wound Clean development in science and technology Co., Ltd production.
After this method is implemented, table 1,2,3 is that the online one-level hydrogenation catalyst the 8th, 9,10 3 days fine de-sulfurs changed respectively is catalyzed Agent groove outlet detection data, are percentage by volume.
Table 1：8th day fine de-sulfur Monitoring Data
Sulfur H2S COS Methyl mercaptan CS2 Thiophene
Pre- desulfurizer 2 18.64 Do not measure 21.66 2.77
Pre- hydrogenation groove 180 3.8 2.42 2.92 3.21
Middle temperature zinc oxide bath B 5 0.15 2.1 0.81 1.6
Middle temperature zinc oxide bath A Do not measure Do not measure Do not measure Do not measure 0.12
Middle temperature zinc oxide bath C Do not measure Do not measure Do not measure Do not measure Do not measure
Secondary hydrogenation groove Do not measure Do not measure Do not measure Do not measure Do not measure
Zinc oxide bath A Do not measure Do not measure Do not measure Do not measure Do not measure
Zinc oxide bath B Do not measure Do not measure Do not measure Do not measure Do not measure
Table 2：9th day fine de-sulfur Monitoring Data
Sulfur H22S COS Methyl mercaptan CS2 Thiophene
Pre- desulfurizer 3 18.48 Do not measure 20.30 2.57
Pre- hydrogenation groove 125 3.7 2.85 0.25 1.33
Middle temperature zinc oxide bath B 3 0.15 2.1 Do not measure 1.00
Middle temperature zinc oxide bath A Do not measure Do not measure 1.71 Do not measure 0.92
Middle temperature zinc oxide bath C Do not measure Do not measure Do not measure Do not measure 0.13
Secondary hydrogenation groove Do not measure Do not measure Do not measure Do not measure Do not measure
Zinc oxide bath A Do not measure Do not measure Do not measure Do not measure Do not measure
Zinc oxide bath B Do not measure Do not measure Do not measure Do not measure Do not measure
Table 3：10th day fine de-sulfur Monitoring Data
Sulfur H2S COS Methyl mercaptan CS2 Thiophene
Pre- desulfurizer 2.8 17.5 11.36 15.01 2.63
Pre- hydrogenation groove 100 16.83 2.02 14.67 2.60
Middle temperature zinc oxide bath B 50 4.04 Do not measure 1.58 2.29
Middle temperature zinc oxide bath A Do not measure 2.01 Do not measure 0.26 Do not measure
Middle temperature zinc oxide bath C Do not measure Do not measure Do not measure 0.10 1.30
Secondary hydrogenation groove Do not measure Do not measure Do not measure 0.09 Do not measure
Zinc oxide bath A Do not measure Do not measure Do not measure Do not measure Do not measure
Zinc oxide bath B Do not measure Do not measure Do not measure Do not measure Do not measure
In the time that one-level hydrogenation catalyst is changed it can be seen from table 1-3, fine de-sulfur outlet sulfur content is complied fully with will Ask.

Claims (7)

1. a kind of method for changing one-level hydrogenation catalyst in coke-stove gas methanol device, it is characterised in that it uses following Method and step：（1）By each filter stop successively and by filler replacement be wood activated charcoal oil absorbent；
（2）Groove parking will be hydrogenated with advance, change the catalyst for pre-hydrogenation in it；
（3）One-level is hydrogenated with to first after groove middle temperature zinc oxide bath parking, the catalyst change iron of middle temperature zinc oxide bath filling Manganese desulphurization catalyst；
（4）One-level is hydrogenated with to second after groove middle temperature zinc oxide bath parking, change the outfit iron molybdenum hydrogenation catalyst on its upper strata；
（5）By one-level hydrogenation groove parking, change and be incorporated to system after one-level hydrogenation catalyst and vulcanized online.
2. the method according to claim 1 for changing one-level hydrogenation catalyst in coke-stove gas methanol device, its feature It is：The step（2）In, the loadings standard of catalyst for pre-hydrogenation is, 5000~6000NM of catalyst space velocities3/m3·h。
3. the method according to claim 1 for changing one-level hydrogenation catalyst in coke-stove gas methanol device, its feature It is：The step（3）In, the loadings standard of ferrimanganic desulphurization catalyst is, 500~700NM of catalyst space velocities3/m3·h。
4. the method according to claim 1 for changing one-level hydrogenation catalyst in coke-stove gas methanol device, its feature It is：The step（4）In, the loadings standard for the hydrogenation catalyst that changes the outfit is, 5000~6000NM of catalyst space velocities3/m3·h。
5. the method according to claim 1 for changing one-level hydrogenation catalyst in coke-stove gas methanol device, its feature It is：The step（1）In, wood activated charcoal oil absorbent is HT-203 activated carbon oil absorbents.
6. change one-level hydrogenation catalyst in coke-stove gas methanol device according to claim 1-5 any one Method, it is characterised in that：The step（1）Before, by adjusting the doctor solution internal circulating load of the wet desulfurization workshop section in upstream, workshop section is improved Export hydrogen sulfide in coke oven content.
7. the method according to claim 6 for changing one-level hydrogenation catalyst in coke-stove gas methanol device, its feature It is：Workshop section outlet hydrogen sulfide in coke oven content is improved to 90~110mg/NM3。
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1277721A2 (en) * 2001-07-19 2003-01-22 Mitsubishi Heavy Industries, Ltd. Method of manufacturing methanol
CN102719289A (en) * 2012-06-21 2012-10-10 新地能源工程技术有限公司 Process for preparing liquefied natural gas (LNG) and hydrogen from coke oven gas
CN104624197A (en) * 2015-01-30 2015-05-20 武汉科林精细化工有限公司 Deoxygenating and desulfurization double-function fine desulfurization agent and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1277721A2 (en) * 2001-07-19 2003-01-22 Mitsubishi Heavy Industries, Ltd. Method of manufacturing methanol
CN102719289A (en) * 2012-06-21 2012-10-10 新地能源工程技术有限公司 Process for preparing liquefied natural gas (LNG) and hydrogen from coke oven gas
CN104624197A (en) * 2015-01-30 2015-05-20 武汉科林精细化工有限公司 Deoxygenating and desulfurization double-function fine desulfurization agent and preparation method thereof

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