CN106635163A - Method for preparing ethylene cracking material from dry coke gas through hydrogenation - Google Patents
Method for preparing ethylene cracking material from dry coke gas through hydrogenation Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G70/00—Working-up undefined normally gaseous mixtures obtained by processes covered by groups C10G9/00, C10G11/00, C10G15/00, C10G47/00, C10G51/00
- C10G70/02—Working-up undefined normally gaseous mixtures obtained by processes covered by groups C10G9/00, C10G11/00, C10G15/00, C10G47/00, C10G51/00 by hydrogenation
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Abstract
The invention discloses a method for preparing an ethylene cracking material from a dry coke gas through hydrogenation. The method comprises the following steps: eluting the dry coke gas with amino so as to remove H2S, CO2 and coke powder, and passing the dry coke gas through a reactor from top to bottom, wherein the following equipment and packing layers are sequentially arranged inside the reactor from top to bottom: a feeding tube, a fed gas distributor, a protection layer, a dearsenic catalyst layer, a hydrogenation catalyst layer, a cold hydrogen feeding tank, a gas distribution layer, a desulfurizing agent layer, a CO and CO2 methanation catalyst layer, a support layer and a discharge tube; packing of the protection layer and the gas distribution layer is selected from at least one of a hydrogenation protection agent and inert packing; the support layer is filled with the inert packing. According to the method disclosed by the invention, one reactor is adopted for hydrogenation at one time, and the situation that one more reactor is added for methanation catalysis for CO and CO2 can be avoided, so that the investment can be reduced, and the procedures can be shortened; due to the arrangement of the cold hydrogen feeding tank and the gas distribution layer, two times of distribution of reaction raw materials can be achieved, the reaction can be relatively complete, and the adaptability of the whole set of device to raw material fluctuation can be improved.
Description
Technical field
The present invention relates to low-carbon alkene hydroprocessing technique, is a kind of method by coking dry gas preparing ethylene cracking material by hydrogenation more specifically.
Background technology
The raw material that China's ethylene unit initial designs are used is based on naphtha.Ethylene raw is the main factor for affecting thylene cost, and raw material proportion in totle drilling cost is 70%～75%.In recent years, Domestic Petrochemical Enterprises were newly-built, extended the large-scale ethylene producing device of many sets, although raw material sources, but ethylene cracking material or pretty nervous have been widened in actual production.In addition, in recent years several next, crude oil price rises steadily, and ethylene cracking material naphtha price is also increased, and enterprise's production economy is deteriorated.Realistic situation forces enterprise to find new ethylene raw to solve this problem, coking dry gas（C2Cut）It is exactly one of the effective ways that solve this problem to be hydrogenated with as ethylene raw.
At present, domestic many walks the petroleum chemical enterprise of Integrated Refinery And Petrochemical, existing ethylene unit, also there are the coking dry gas of affluence simultaneously, and rich in ethane and a small amount of ethene in coking dry gas, if wherein a small amount of ethene is carried out into saturated hydrogenation, this coking dry gas is exactly good ethylene raw.
Hydrogenation of olefins in coking dry gas is transformed into alkane, is in theory simple, but many difficult points are had in the specific implementation process of technology, such as, coking dry gas composition has following features：（1）Containing carbon monoxide and carbon dioxide；（2）Sulfur-bearing is higher；（3）While to coking dry gas hydrogenation, hydrogenation depth deoxidation is also wanted, and to reach oxygen content index ≯ 1.0mgm-3.Ethylene cracking material can be done to reach the index in table 1 after coking dry gas process.
The ethylene cracking material index of table 1.
CN1800308A discloses a kind of C2And C2The method that above hydrocarbon component is reclaimed, the method includes following processing routine to dry gas：More than ten operation such as pressure-variable adsorption, amine wash-out sulphur, washing, water separation, fine de-sulfur, dearsenification, fine de-sulfur, deoxidation, alkali cleaning carbon dioxide removal, washing dealkalize, water separation, dealkalize, Adsorbing drying by pressure variation.Although tissue production in this way can obtain ethylene cracking material, production procedure is oversize, and cumbersome, production cost is higher.
For problem present in said method, CN103450941A is improved, it is proposed that a kind of method that coking dry gas prepare ethylene cracking material.The method is raw materials used such as table 2.
The coking dry gas of table 2. are constituted
Note：C2+ is the component of carbon more than two.
Include following processing routine successively to dry gas：
（1）Amine is carried out to coking dry gas to wash；Purpose is to slough H2S、CO2, coke powder.
（2）Coking dry gas are hydrogenated with, it is therefore an objective to deolefination, deoxidation, removing part CO and CO2。
（3）Pressure-variable adsorption is carried out to coking dry gas, it is therefore an objective to collect rich ethane gas.
Table 2 is constituted for the raw material of the production stage of stable development, and it can be the index up to ethylene cracking material to produce its product by above-mentioned production procedure and condition tissue when device is in the stage of stable development.But but it is not that so, raw material fluctuation composition is larger in actual production.It is that two coking towers switch over operation that reason is coking production device, and the process characteristic of 24 hours a cycles, i.e. coking plant determines that inevitably resulting in raw material regularly fluctuates.Raw material fluctuation composition such as table 3 in actual production.
Raw material fluctuation composition in the actual production of table 3.
The selected catalyst of reaction is sulfide type catalyst, has good selectivity to deolefination and deoxidation；To CO and CO2Hydrogenation select it is slightly poor.Under normal production scenarios, CO ≯ 0.40% in raw material, CO2≯0.20%.Under raw material deolefination and the reaction condition of deoxidation, CO and CO2Can have 40% ~ 50% or so to be hydrogenated, the CO not being hydrogenated with and CO2Can be completed by follow-up pressure-variable adsorption workshop section.
The content fluctuation of alkene and oxygen in reaction raw materials can make reaction result reach the technical requirement of product by adjusting reaction temperature；But as CO and CO in reaction raw materials2When content off-design value is higher, it is hydrogenated after CO and CO2Index is also exceeded, this CO and CO2Exceeded material gives follow-up pressure-swing absorption apparatus, it is desirable to be separated off CO and CO by adjusting pressure-swing absorption apparatus2, also will be difficult to.
By to CO and CO2The research of hydrogenation reaction knows that the catalyst used by CN103450941A is the sulfide type catalyst of Wu-Mo, and such catalyst has selective well to hydrogenation of olefins and oxygen hydrogenation；And to containing CO and CO in raw material simultaneously2, its hydrogenation selectivity it is then poor, reason is：If such catalyst in raw material to only having CO, its hydrogenation selectivity is fine；To there was only CO in raw material2When, its hydrogenation selectivity is poor.CO2There is very strong adsorptivity to the hydrogenation sites of catalyst, in CO and CO2Under the conditions of simultaneous, CO and CO2There is the relation of competitive Adsorption, CO2It is preferentially adsorbed on the hydrogenation sites of catalyst, i.e. CO2Preferential Occupancy phenomenon is shown to CO, hinders CO that the carrying out of hydrogenation reaction occurs, the result that we obtain reacting is exactly, in CO and CO2When coexisting, the two is all difficult to be hydrogenated.
By to CO and CO2The research of hydrogenation reaction know another as a result, in CO and CO2When coexisting, the catalyst that the two is all easily hydrogenated is Ni series catalysts.But such catalyst is afraid of sulphur, if using such catalyst hydrogenation reaction, sulfur content is less than 1.0 mg/m in its raw material3。
The content of the invention
There is component fluctuation in the present invention, especially CO and CO for coking dry gas in prior art actual production2Content off-design value is higher, causes CO and CO in the ethylene cracking material after being hydrogenated with2The problem of index exceeding standard, the present invention devises the production technology that a kind of coking dry gas prepare ethylene cracking material, CO and CO of the method in hydrogenating materials2When content off-design value is higher, the material after hydrogenation can be still set to reach the required index of follow-up pressure-variable adsorption workshop section charging.
The technical purpose of the present invention is realized by below scheme technical scheme：
A kind of method of coking dry gas preparing ethylene cracking material by hydrogenation, the coking dry gas elder generation Jing amine wash-out removes H2S、CO2, coke powder, then from top to bottom by reactor, in reactor following equipment and packing layer are set gradually from top to bottom：Feed pipe, gas feed distributor, protective layer, dearsenification oxidant layer, hydrogenation catalyst oxidant layer, cold hydrogen material feeding box, gas distribution layers, desulfurization oxidant layer, CO and CO2Methanation catalyst oxidant layer, supporting layer and discharge nozzle；
At least one of the filler of the protective layer and gas distribution layers in hydrogenation protecting agent and inert filler, the supporting layer is loaded by inert filler.
The coking dry gas elder generation Jing amine wash-out of composition shown in table 3 removes H2S、CO2, coke powder, its composition is shown in Table 4.
The coking dry gas Jing amine of table 4. wash-out removes H2S、CO2, composition after coke powder
Process by coking dry gas preparing ethylene cracking material by hydrogenation is gas（Coking dry gas）Gu-（Catalyst）Strong exothermal reaction, therefore from from reaction mass transfer, gas distribution is the problem to be paid close attention to of emphasis.Reaction is fed using top, bottom discharging.
Jing amine wash-out first removes H2S、CO2, coke powder coking dry gas, Jing feed pipes enter gas feed distributor, and then by protective layer, the effect of protective layer has two, the distribution of first gas；Its two be absorption or filter material in mechanical admixture.
It is distributed through gas and the coking dry gas of purification continues flow through dearsenification oxidant layer, slough the micro amount of arsenic in material, pass through hydrogenation catalyst oxidant layer, deolefination, deoxygenation is carried out in this bed.Hydrodearsenic Catalyst loadings in the dearsenification oxidant layer are 5.0 v of the hydrogenation catalyst in hydrogenation catalyst oxidant layer
%~10v%。
Material carries out deolefination and deoxygenation in hydrogenation catalyst oxidant layer, and raw material is shown in Table 4, and required condition and reaction result are shown in Table 5.
The suitable reaction condition and result of the coking dry gas of table 5. hydrogenation
Hydrogen partial enters the cold hydrogen material feeding box by feed pipe, because hydrogen contained in initial feed is consumed in the majority after hydrogen catalysis oxidant layer, now injects cold hydrogen, and one is to increase the hydrogen content in material, hydrogen dividing potential drop is improved, beneficial to CO and CO2Next step carries out methanation reaction；It two is that temperature of charge is adjusted to the temperature carried out required for methanation reaction.
The cold hydrogen newly come in cold hydrogen material feeding box realizes preliminary mixed distribution with raw material, hydrogen further to make new injection is well mixed with original material, so that methanation reaction carry out it is more complete, only come what distributing hydrogen still fell flat by cold hydrogen material feeding box, from in the distribution of hydrogen with immixture, cold hydrogen material feeding box Main Function is to stress Hydrogen distribution, secondary role is to complete the mixing of a gas, so to make newly to inject hydrogen being well mixed before into methanation reaction bed with original material, it is necessary to carry out quadratic distribution and mix.The setting of gas distribution layers is exactly to complete the quadratic distribution of gas.
The function setting of protective layer in accordance with the above and gas distribution layers, available filler scope is widely in two layers.For example：Hydrogenation reaction behind for the benefit of, may be selected active filler, the hydrogenation protecting agent being such as suitable in this area；Variously-shaped inert filler is also may be selected, entity filler or gauze packing can meet requirement.Used as the technical scheme of optimization, the inert filler in the present invention preferably is selected from least one in inert ceramic balls, Bird's Nest proppant and ceramic honey comb.
Further, a diameter of Φ 13mm ~ 20mm of the filler of the protective layer, its filling height is 100 ~ 600mm, more preferably 200 ~ 500mm.
Further, the gas distribution layers are formed by the filling of at least 3 kinds fillers, described filler by the descending order of particle diameter in reactor by from top to bottom arranging.From the aspect of the mass transfer for chemically reacting, this is conducive to gas mixing uniform.From from the point of view of the requirement and saving of whole production technology, the gas distribution layers are preferably formed by 3 kinds of fillers fillings, and a diameter of Φ 13mm ~ 20mm of filler of wherein ground floor, the second layer is Φ 6mm ~ 8mm, and third layer is Φ 4mm ~ 2mm.
Further, the filling of every kind of filler is highly 200 ~ 600mm in the gas distribution layers.It is 200 ~ 500mm that the filling of wherein ground floor is highly preferred, and it is 300 ~ 500mm that the filling of the second layer is highly preferred.
Due to current existing CO and CO2Methanation catalyst is Ni types, such catalyst not resistant to sulfur, typically to make sulfur content of raw material less than 1.0ppM, and desulfurization oxidant layer is arranged for this.
The reaction condition of material is shown in Table 6. in desulfurization oxidant layer
The suitable reaction condition of the coking dry gas of table 6. absorption desulfurization and result
After the above treatments material enters into CO and CO2In methanation catalyst oxidant layer, methanation reaction can be completed, required condition and reaction result are shown in Table 7.
The .CO of table 7 and CO2The suitable reaction condition of methanation reaction and result
The supporting layer is loaded by inert filler, and mainly the filler and catalyst to loading in whole reactor is played a supporting role.
Various Hydrodearsenic Catalysts used, desulfurizing agent and catalyst can be the product of the function of commercially available achievable application claims in the present invention.Such as Hydrodearsenic Catalyst can be FDAs-1, and the hydrogenation catalyst can select LH-10A, and desulfurizing agent is the adsorption desulfurizing agent of ZnO types, and methanation catalyst is J108Q of selection commercialization etc..
Beneficial effects of the present invention：
The present invention adopts a step hydrogenation reaction using coking dry gas, not only completes deolefination, deoxidation, while completing the de- CO and CO of depth2；It is used for CO and CO with a reactor is increased in addition2Methanation catalyst is compared, and using a hydrogenation reactor, is reduced investment outlay, and also shortens flow process, simplifies operation；The distribution twice of reaction raw materials is realized by arranging cold hydrogen material feeding box and gas distribution layers, the reaction after being allowed to is more complete, increased the adaptability that package unit fluctuates to raw material, i.e., as the CO and CO in reaction raw materials2When content off-design value is higher, it is hydrogenated after CO and CO2Index can also reach the index of raw material required for pressure-swing absorption apparatus, and then ensure that pressure-swing absorption apparatus produces qualified ethylene cracking material.
Specific embodiment
Following non-limiting examples can make one of ordinary skill in the art that the present invention is more fully understood, but limit the present invention never in any form.
Embodiment
1
Following equipment and packing layer are from top to bottom set gradually in reactor：Feed pipe, gas feed distributor, protective layer, dearsenification oxidant layer, hydrogenation catalyst oxidant layer, cold hydrogen material feeding box, gas distribution layers, desulfurization oxidant layer, CO and CO2Methanation catalyst oxidant layer, supporting layer and discharge nozzle.Wherein protective layer is the Bird's Nest proppant of Φ 13, and its filling height is 300mm.Dearsenification oxidant layer is FDAs-1 Hydrodearsenic Catalysts, it is LH-10A hydrogenation catalysts in hydrogenation catalyst oxidant layer, gas distribution layers are formed by 3 kinds of filler fillings, the inert ceramic balls of the Bird's Nest proppant, the inert ceramic balls of Φ 6 and Φ 3 of Φ 13 are from top to bottom respectively, wherein each layer height is followed successively by 400mm, 300mm, 300mm.Desulfurizing agent is the adsorption desulfurizing agent of ZnO types, and methanation catalyst is the J108Q of commercialization.
Coking dry gas elder generation Jing amine wash-out is removed into H2S、CO2, coke powder, from top to bottom by reactor, tissue production.Raw materials used composition is shown in Table 8, reaction condition and the results are shown in Table 9.
The coking dry gas Jing amine of table 8. wash-out removes H2S、CO2, composition after coke powder
The coking dry gas hydrogenation and olefin hydrocarbon removal of table 9., the reaction condition of deoxidation and result
Material after the hydrogenated deolefination of coking dry gas, deoxygenation its reaction condition and the results are shown in Table 10 through desulfurization oxidant layer.
The reaction condition and result of the coking dry gas of table 10. absorption desulfurization
Material after desulfurization Jing CO and CO again2Methanation catalyst oxidant layer, its reaction condition and result are listed in table 11.
The coking dry gas of table 11. Jing methanation reactions condition and result again
Knowable to the data in table 11, in table 8 after the hydrogenated deolefination of material and deoxygenation, then Jing after methanation reaction, olefin(e) centent, oxygen content in product, CO, CO2Content reached the technical requirement for doing ethylene cracking material.
Comparative example
1
A setting feed pipe, gas feed distributor, protective layer, dearsenification oxidant layer, hydrogenation catalyst oxidant layer, gas distribution layers and discharge nozzle in reactor; the filler for wherein loading in protective layer and gas distribution layers and height are with embodiment 1; carry out the production of coking dry gas preparing ethylene cracking material by hydrogenation; it is raw materials used also as shown in table 8, reaction condition and the results are shown in Table 12.
The reaction condition and result of the coking dry gas of table 12. hydrogenation
Knowable to the data in table 12, in table 8 after the hydrogenated deolefination of material and deoxygenation, the olefin(e) centent and oxygen content in product has reached the technical requirement for doing ethylene cracking material, but this hydrogenation process only has the CO and CO of part2It is hydrogenated, so this two technical indicators are also not up to the technical indicator required by ethylene cracking material.
Send next operation in table 8 after the hydrogenated deolefination of material and deoxygenation, pressure-variable adsorption workshop section, the argument that pressure-variable adsorption workshop section is arranged is point to be enriched with ethane except methane, and secondary work(is point to remove CO and CO2, and pressure-variable adsorption is to CO and CO2Divide except rate highest only has 95%, generally divide except rate is 90%, so the results are shown in Table 13 after this treatment.
Coking dry gas after the hydrogenation of table 13. result again Jing after pressure-variable adsorption
From the data in table 13, coking dry gas after this treatment, CO and CO2Content be exceed ethylene cracking material required by technical indicator, fail to reach requirement.
Comparative example
2
Inside reactor bed is loaded compared with embodiment, and its difference is to be not provided with gas distribution layers, and others are arranged and operated same as Example 1.
Coking dry gas elder generation Jing amine wash-out is removed into H2S、CO2, coke powder, from top to bottom by reactor, tissue production.Raw materials used composition is shown in Table 8, reaction condition and the results are shown in Table 14.
The coking dry gas hydrogenation and olefin hydrocarbon removal of table 14., the reaction condition of deoxidation and result
Material after the hydrogenated deolefination of coking dry gas, deoxygenation its reaction condition and the results are shown in Table 15 through desulfurization oxidant layer.
The reaction condition and result of the coking dry gas of table 15. absorption desulfurization
Material after desulfurization Jing CO and CO again2Methanation catalyst oxidant layer, its reaction condition and result are listed in table 16.
The coking dry gas of table 16. Jing methanation reactions condition and result again
Knowable to the data in table 16, in table 8 after the hydrogenated deolefination of material and deoxygenation, then Jing after methanation reaction, it is 0.71 mgm that the olefin(e) centent in product is 0.17mol%, oxygen content-3, sulfur content be 0.65
mg·m-3, these indexs reach the technical requirement of ethylene cracking material；But at this point in the reaction, CO, CO2Content be respectively 990 mgm-3With 570 mgm-3, the two indexs fail the technical requirement for reaching ethylene cracking material, illustrate to be not provided with gas distribution layers in reaction bed, will result in hydrogen（The hydrogen come in by cold hydrogen box）Initial mixing and skewness, and hydrogen initial distribution inequality can make methanation catalyst effect reduce by 30% or so.
Claims (9)
1. a kind of method of coking dry gas preparing ethylene cracking material by hydrogenation, it is characterised in that the coking dry gas elder generation Jing amine wash-out removes H2S、CO2, coke powder, then from top to bottom by reactor, in reactor following equipment and packing layer are set gradually from top to bottom：Feed pipe, gas feed distributor, protective layer, dearsenification oxidant layer, hydrogenation catalyst oxidant layer, cold hydrogen material feeding box, gas distribution layers, desulfurization oxidant layer, CO and CO2Methanation catalyst oxidant layer, supporting layer and discharge nozzle；
At least one of the filler of the protective layer and gas distribution layers in hydrogenation protecting agent and inert filler, the supporting layer is loaded by inert filler.
2. method according to claim 1, it is characterised in that at least one of the inert filler in inert ceramic balls, Bird's Nest proppant and ceramic honey comb.
3. method according to claim 1, it is characterised in that the gas distribution layers are formed by least 3 kinds fillers fillings, described filler by the descending order of particle diameter in reactor by from top to bottom arranging.
4. method according to claim 3, it is characterised in that the gas distribution layers are formed by 3 kinds of fillers fillings, a diameter of Φ 13mm ~ 20mm of filler of wherein ground floor, the second layer is Φ 6mm ~ 8mm, and third layer is Φ 4mm ~ 2mm.
5. method according to claim 3, it is characterised in that the filling of every kind of porcelain ball in the gas distribution layers is highly 200 ~ 600mm.
6. method according to claim 1, it is characterised in that a diameter of Φ 13mm ~ 20mm of filler of the protective layer, filling height is 100 ~ 600mm.
7. method according to claim 1, it is characterised in that the operating condition when coking dry gas flow through reaction in hydrogenation catalyst oxidant layer is：120 ~ 300 DEG C of inlet temperature, 1.0 ~ 6.0MPa of pressure, volume of material 100 ~ 1000/h of air speed-1, 220 ~ 380 DEG C of outlet temperature.
8. method according to claim 1, it is characterised in that it is 1000 ~ 4000/h that the coking dry gas flow through the volume of material air speed of desulfurization oxidant layer-1。
9. method according to claim 1, it is characterised in that the coking dry gas flow through CO and CO2In methanation catalyst oxidant layer react when operating condition be：250 ~ 350 DEG C of inlet temperature, 0.5 ~ 6.0MPa of pressure, volume of material 6000 ~ 10000/h of air speed-1。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110129088A (en) * | 2019-05-06 | 2019-08-16 | 盘锦北方沥青燃料有限公司 | A kind of method of lower carbon number hydrocarbons mixed hydrogenation production ethylene cracking material |
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| CN203295451U (en) * | 2013-06-03 | 2013-11-20 | 北京燕山玉龙石化工程有限公司 | Ethane-rich dry gas purifying and refining device |
| CN103450941A (en) * | 2012-05-30 | 2013-12-18 | 中国石油化工股份有限公司 | Method for producing ethylene cracking raw material from coking dry gas |
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| CN1415532A (en) * | 2001-11-01 | 2003-05-07 | 中国石化工程建设公司 | Method for preparing high purity hydrogen by catalyzing dry gas being as raw material |
| US20100249474A1 (en) * | 2009-03-31 | 2010-09-30 | Nicholas Christopher P | Process for Oligomerizing Dilute Ethylene |
| CN103450941A (en) * | 2012-05-30 | 2013-12-18 | 中国石油化工股份有限公司 | Method for producing ethylene cracking raw material from coking dry gas |
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| CN110129088A (en) * | 2019-05-06 | 2019-08-16 | 盘锦北方沥青燃料有限公司 | A kind of method of lower carbon number hydrocarbons mixed hydrogenation production ethylene cracking material |
| CN110129088B (en) * | 2019-05-06 | 2021-03-30 | 盘锦北方沥青燃料有限公司 | Method for producing ethylene cracking raw material by low-carbon hydrocarbon mixed hydrogenation |
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Effective date of registration: 20230825 Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee after: CHINA PETROLEUM & CHEMICAL Corp. Patentee after: Sinopec (Dalian) Petrochemical Research Institute Co.,Ltd. Address before: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee before: CHINA PETROLEUM & CHEMICAL Corp. Patentee before: DALIAN RESEARCH INSTITUTE OF PETROLEUM AND PETROCHEMICALS, SINOPEC Corp. |
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