CN1075740A - Oil refinery dry gas and the charging of petroleum naphtha mixed phase are produced hydrogen, methane, carbon monoxide, the method for carbonic acid gas from hydrofining - Google Patents
Oil refinery dry gas and the charging of petroleum naphtha mixed phase are produced hydrogen, methane, carbon monoxide, the method for carbonic acid gas from hydrofining Download PDFInfo
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- CN1075740A CN1075740A CN 92111165 CN92111165A CN1075740A CN 1075740 A CN1075740 A CN 1075740A CN 92111165 CN92111165 CN 92111165 CN 92111165 A CN92111165 A CN 92111165A CN 1075740 A CN1075740 A CN 1075740A
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Abstract
The present invention relates to the by product of refinery---the development and use of oil refinery dry gas.Oil refinery dry gas removes wherein hydrogen sulfide, carbon monoxide, carbonic acid gas through diethanolamine, through the oil refinery dry gas behind gas-liquid separation, the separatory is compressed boost after, with the charging of petroleum naphtha mixed phase, oil refinery dry gas is the interior adjusting arbitrarily of 20～80% (wt) scope of mixed phase charging, through hydrofining, desulfurization, deep refining, make the hydrocarbon flow behind the mixed phase become good steam reforming charging, generate hydrogen, methane, carbon monoxide, carbonic acid gas through conversion reaction, provide cost-effective method for further producing synthetic ammonia, methyl alcohol, steam, hydrogen etc.
Description
The present invention relates to the development and use of the by product-oil refinery dry gas (also claiming hydrocarbon gas) in the oil refining courses of processing such as refinery catalytic cracking, thermally splitting, coking, reformation, visbreaking and catalytic pyrolysis.
The major ingredient of oil refinery dry gas is by H
2, CH
4, C
2H
4, C
2H
6, C
3H
6, C
3H
8, CO, CO
2, H
2S and a spot of C
4, C
5Deng composition.Existing most of oil refinery dry gas is not exploited, and burns mainly as fuel gas, and is very unfortunate.If can be with oil refinery dry gas through suitable processing, by the hydrogen in the oil refinery dry gas from hydrofining, Alkene hydrogenation wherein is saturated, sulphur etc. remove, in order to replace or partly to replace petroleum naphtha, generate hydrogen, methane, carbon monoxide, carbonic acid gas through steam reforming reaction, become the valuable industrial chemicals of further production synthetic ammonia, methyl alcohol, hydrogen etc.This deep processing and resource optimization for oil will be highly significant.Since the seventies oil crisis, the naphtha resource shortage, price increase is that the synthetic ammonia installation of raw material is sought raw material as an alternative such as the more cheap Sweet natural gas of price, liquefied gas, oil refinery dry gas one after another with light oil.
Utilize the hydrogen in the oil refinery dry gas production ammonia synthesis gas, now mainly contain four kinds of methods: first kind is adopted partial oxidation process, and this method need be built air separation facility and be supplied with oxygen rich gas, and its investment is big, the energy consumption height, and catalyst carbon deposition is serious; Select anti-conversion of olefines catalyzer for use for second kind, the easy carbon distribution of catalyzer, active low, coil damage is serious, and the operational cycle is short; The third selects the single alkane of component for use, and this method need be set up gas separation unit (mainly being that the alkane in the hydrocarbon gas and rare hydrocarbon are separated), and the alkane in the gas separation unit is used as converted feed; The 4th kind of hydro-refining unit that adopts self-organizing system beaten the cycle control reaction temperature rising with the fine gas cooling, and this method need increase special cycle heat exchange equipment, and energy utilizes unreasonable.
The objective of the invention is to avoid above-mentioned weak point of the prior art, a kind of tripping device that do not need is provided, reduced investment, employing oil refinery dry gas that energy consumption is low and the charging of petroleum naphtha mixed phase are from hydrofining, become good steam and change charging, generate hydrogen, methane, carbon monoxide, the economy of carbonic acid gas, effective means through steam reforming reaction.
Task of the present invention is achieved in that as Fig. 1 oil refinery dry gas process diethanolamine removes H wherein
2S, CO, CO
2Behind sour gas, through gas-liquid separation, compression, after the charging of petroleum naphtha mixed phase, preheating; Carry out hydrofining then, will contain 10～20%(V) Alkene hydrogenation to be saturated to＜1%(V), COS, RSH etc. changes into H
2S, again through the ZnO desulfurization, total sulfur is reduced to＜0.5ppm, deep fat air-flow after the desulfurization and the heat exchange of cold oil air-flow are cooled to about 200 ℃, deep refining through high-nickel catalyst, can with the aromatic hydrocarbons in the petroleum naphtha by 10～20%(wt) reduce to＜1%(wt), the alkene in the oil refinery dry gas is reduced to the ppm level, the sulphur in the hydrocarbon flow, chlorine, arsenic are reduced to the ppb level.Like this, after oil refinery dry gas and the charging of petroleum naphtha mixed phase,, enter the steam reforming reaction operation, generate hydrogen, methane, carbon monoxide, carbonic acid gas through above-mentioned operation.
The drawing of accompanying drawing is described as follows:
Fig. 1 is a process flow diagram of the present invention.Among the figure: (1) oil refinery dry gas, (2) diethanolamine removes the sour gas operation, (3) gas-liquid separation operation, (4) compression section, (5) oil refinery dry gas and petroleum naphtha mixed phase, benefit hydrogen operation, (6) preheating procedure (with hot hydrocarbon flow heat exchange heating process, with cold conditions hydrocarbon flow heat exchange cooling process), (7) hydrofining operation, (8) zinc oxide separation of flow operation, (9) degree of depth Seiko preface, (10) heating process, (11) steam reforming reaction operation.
* mend the effect of hydrogen:
1. hydrogen richness is on the low side sometimes in the oil refinery dry gas, guarantee hydrogen/alkene mol ratio＞1.10
2. the petroleum naphtha hydrogenation refining desulfurization needs hydrogen
3. the petroleum naphtha aromatic hydrogenation is saturated in the deep refining need consumption hydrogen
4. for guaranteeing that steam reforming reaction normally carries out, need to replenish necessary hydrogen
Fig. 2 is a process flow sheet of the present invention.Among the figure: (1) diethanolamine washing tower, (2) knockout drum, (3) compressor, (4) interchanger, (5) process furnace, (6) hydrogenator, (7) zinc oxide desulfurization reactor, (8) deep refining reactor, (9) naphtha feed pump, (10) knockout drum, (11) interchanger, (12) process furnace, (13) naphtha tank.(A) diethanolamine liquid, (B) sulfur-bearing washings, (C) oil refinery dry gas, (D) remove oil refinery dry gas behind the sour gas, (E) parting liquid (diethanolamine liquid) (F) (is used as) fuel gas, (G) (be used as) unstripped gas, (Y) advance the circulation fine gas of compressor, the unstripped gas after (H) boosting, (I) hydrogen make-up, (J) petroleum naphtha, (V) hydrocarbon flow behind the mixed phase, (K) hydrocarbon flow after the heat exchange, (L) hydrocarbon flow after the preheating, (M) hydrocarbon flow behind the hydrogenation, (N) hydrocarbon flow behind the zinc oxide desulfurization, (X) hydrocarbon flow after the cooling, (P) hydrocarbon flow behind the deep refining, (Q) hydrocarbon flow after the heating, enter the steam reforming reaction operation, generate hydrogen, methane, carbon monoxide, carbonic acid gas, (W) cooled circulation fine gas.
The present invention 2 is described in further detail in conjunction with the accompanying drawings:
The composition more complicated of oil refinery dry gas has H
2, N
2, H
2S, CH
4, C
2H
4, C
2H
6, C
3H
6, C
3H
8, CO, CO
2, RSH, COS and a spot of C
4, C
5, H
2O etc. see table 1 for details.
With oil refinery dry gas (C) through diethanolamine washing tower (1) will be wherein H
2S, CO, CO
2Take off to＜1%(V), remove oil refinery dry gas (D) the air inlet liquid separating tank (2) behind the sour gas, oil refinery dry gas behind the separatory is divided into two portions, the part gas (F) that acts as a fuel, a part is refining with unstripped gas (G) as the steam reforming charging, the compressed machine of unstripped gas (G) (3) boosts, unstripped gas after boosting (H) (is hydrogen/rare mol ratio of assurance oil refinery dry gas hydrogenation with hydrogen make-up (I), the petroleum naphtha aromatic hydrogenation is saturated with hydrogen etc. in hydrodesulfurizationof of naphtha and the deep refining) and petroleum naphtha (J) boost through pump (9), (H), (I), (J) hydrocarbon flow (N) after mixed hydrocarbon flow of three (V) (being oil refinery dry gas and the charging of petroleum naphtha mixed phase) and the hydrofining is in interchanger (4) heat exchange, hydrocarbon flow after the heat exchange (K) enters process furnace (5) preheating, hydrocarbon flow after the preheating (L) enters hydrogenator (6) (filling 481-3 or CH-6 catalyzer in the device), the Alkene hydrogenation of 10～20%(V) in the oil refinery dry gas is saturated, make total olefin＜1%(V), COS, RSH is hydroconverted into H
2S.Hydrocarbon flow behind the hydrogenation (M) enters zinc oxide desulfurization reactor (7), through zinc oxide desulfurization, with H
2S changes into ZnS, makes the total sulfur＜0.5ppm in the hydrocarbon flow.Through the deep fat air-flow (N) behind the zinc oxide desulfurization and cold oil air-flow (V) heat exchange in interchanger (4), be cooled to hydrocarbon flow (X) separated into two parts about 200 ℃: in the scope of hydrogenator (6) service temperature permission, the whole or most of of hydrocarbon flow (X) can be carried out deep refining through deep refining reactor (8) (filling 0501 high-nickel catalyst in the device), can be with detrimental impurity sulphur (S) wherein, chlorine (CL), arsenic (As) etc. takes off the level to ppb, alkene in the oil refinery dry gas is reduced to the ppm level, with the aromatic hydrocarbons in the petroleum naphtha by 10～20%(wt) reduce to＜1%(wt), become good steam reforming charging-hydrocarbon flow (P).Hydrocarbon flow (P) enters process furnace (12) and is heated to about 380 ℃-hydrocarbon flow (Q), and hydrocarbon flow (Q) is mixed laggard converter and carried out steam reforming reaction with water vapor, generates hydrogen, methane, carbon monoxide, carbonic acid gas; When the blending proportion of oil refinery dry gas and petroleum naphtha higher, when the highest bed temperature of hydrogenator (6) surpasses tolerance band, can from hydrocarbon flow (X), draw the part hydrocarbon flow through the further cooling-hydrocarbon flow (W) of interchanger (11), and behind gas-liquid separator (10) separatory hydrocarbon flow (Y), advance compressor (3) and play circulation, as the means of regulating hydrogenator (6) bed temperature, also available this loop is as the loop of carrying out closed cycle under start-stop car or the accidental state.
The steam reforming reaction of hydro carbons carries out under 500～800 ℃ usually, C
2Above hydro carbons all will generate this stage of methane through cracking, scission of link.Methane again with H
2The O reaction generates H
2, CO, CO
2Cracking, dehydrogenation, condensation at high temperature very easily take place, analyse reaction, particularly alkene and aromatic hydrocarbons such as carbon in hydro carbons, are more prone to analyse carbon.Therefore, prevent that the carbon distribution of hydro carbons on conversion catalyst from being the conversion process operation
In matter of utmost importance.Usually requiring alkene ≯ 1%(wt), aromatic hydrocarbons ≯ 13%(wt), petroleum naphtha does ≯ and 220 ℃.Alkene in the oil refinery dry gas is generally 10～20%(V).So the present invention, must be saturated to the hydrogenation of olefins in the oil refinery dry gas＜1%(V), could satisfy the requirement of steam reforming charging before advancing the steam reforming stove oil refinery dry gas.For this reason, the present invention utilizes in the oil refinery dry gas contained 18～30%(V) hydrogen (from hydrogenation) that its hydrogenation of olefins of contained 10～20%(V) is saturated.
Hydrogenation of olefins is saturated to be strong exothermal reaction.So it is crucial preventing oil refinery dry gas overtemperature in hydrogenator (6).The service temperature of Hydrobon catalyst ≯ 380 ℃, the saturated a large amount of heats of emitting of ethene and propylene hydrogenation in the oil refinery dry gas, as not taking the heat exchange measure, reaction bed temperature is risen to rapidly more than 500 ℃, cause the rapid carbon distribution inactivation of catalyzer, the accident that also can cause jeopardizing production safety takes place.For guaranteeing that catalyzer is in the high reactivity state in the whole production cycle, often adopts the state of operation of low temperature high activity.The present invention petroleum naphtha as heat-absorbing medium, with petroleum naphtha and the charging of oil refinery dry gas mixed phase, utilize the big characteristics of petroleum naphtha vaporization heat, be easy to beds is controlled in the scope of permission, the amount of oil refinery dry gas can be the interior adjusting arbitrarily of 20～80%(wt) scopes of whole mixed phase inlet amount.
The processing condition of hydrogenator of the present invention (6) are:
Temperature of reaction: 180～380 ℃
Reaction pressure: 1.0～4.5MPa
Oil refinery dry gas reaction gas air speed: 500～3000h
-1
Petroleum naphtha liquid air speed: 0.5～4.0h
-1
Hydrogen/alkene mol ratio:＞1.10
Charging sulfur-bearing: ≮ 3ppm
Catalyzer: cobalt-molybdenum, nickel-molybdenum or nickel-molybdenum-tungsten is the Hydrobon catalyst of active ingredient, first-selected CH-6,481-3.
The hydrocarbon steam conversion method is that hydrocarbon gas and petroleum naphtha are the most economical method of the production synthetic ammonia or the hydrogen of raw material.It has without oxygen and reduced investment, advantage of low energy consumption.
The hydrocarbon steam conversion method has strict requirement to the charging of hydro carbons.Except that the alkene in the charging, aromatic hydrocarbons, raw material being done strict requirement, detrimental impurity sulphur, chlorine, arsenic wherein also there is the requirement of strictness.
Conversion catalyst is a nickel catalyst.In the conversion reaction, be to be active ingredient with the nickel of going back ortho states.Arsenic in the hydro carbons is its permanent poison, and the sulfide in the hydro carbons, muriate all are converted into H under 500～800 ℃ the condition that hydrogen exists
2S, HCI, and generate NiS, NiCl with nickel reactant in the catalyzer
2, causing the poisoning of catalyst inactivation, present hydrodesulfurizationof of naphtha both domestic and external (ZnO) technology can only be taken off sulphur, chlorine the level to ppm, and aromatic hydrocarbons is constantization substantially.Adopt deep refining technology of the present invention, not only alkene can be taken off level to ppm, aromatic hydrocarbons take off to＜1%(wt), and sulphur, chlorine, arsenic can be taken off level to ppb, this keeps high reactivity for a long time to improving the throughput of conversion catalyst, and reducing operating severity has crucial meaning.
The processing condition of zinc oxide desulfurization reactor of the present invention (7):
Reaction stagnation pressure: 1.0～4.5MPa
Temperature of reaction: 250～400 ℃
Gas air speed: 500～3000h
-1
The liquid air speed of petroleum naphtha: 0.5～2.0h
-1
The processing condition of deep refining reactor of the present invention (8) are:
Reaction stagnation pressure: 1.0～4.0MPa
Temperature of reaction: 140～240 ℃
Oil refinery dry gas gas air speed: 500～3000h
-1
The liquid air speed of petroleum naphtha: 0.5～2.0h
-1
Catalyzer: high-nickel catalyst, first-selected 0501 catalyzer.
The processing condition of steam reforming reaction of the present invention are:
Reaction pressure: 1.0～4.5MPa
Temperature in: 450～500 ℃
Temperature out: 750～800 ℃
1/3 bed temperature: ≯ 630 ℃
Oil refinery dry gas gas air speed: 500～1000h
-1
Petroleum naphtha liquid air speed: 0.5～1.0h
-1
Steam/hydrocarbons ratio: 3.0～4.5
Catalyzer: RKNR or Z409/Z405
The present invention has following advantage than prior art:
1. utilize the big characteristics of petroleum naphtha vaporization heat, with it as heat-absorbing medium.Like this, petroleum naphtha and the charging of oil refinery dry gas mixed phase are controlled at reaction bed temperature in the scope of permission easily.Can guarantee production equipment operation steady in a long-term, not need standby reactor, adopt the operation of the low recycle ratio (or not circulating) of low temperature high activity, it is little to have equipment volume, and systemic resistance is little, and heat makes full use of, reduced investment, and energy consumption is low.
2. adopt the deep refining operation, can with in the steam reforming reaction easily material sulphur, chlorine, the arsenic of poisoning carbon distribution take off level to ppb, alkene takes off the level to ppm, aromatic hydrocarbons take off to＜1%(wt).Help prolonging the running period of conversion catalyst, reduce steam/hydrocarbons ratio, improve treatment capacity, energy-saving and cost-reducing.
3. to be specially adapted in the large-scale petroleum chemical enterprise with the petroleum naphtha be that raw material pre-refining before the steam reforming operation of raw material improves in the present invention.Only need do a spot of transformation, can implement the present invention, and obtain remarkable economic efficiency and social benefit.
Annotate: expression gas %(V), liquid or gas-liquid mixture %(wt) expression.
Annotate: table 1 is formed for the oil refinery dry gas that removes behind the sour gas.
Claims (10)
1, a kind of refinery's thousand gas and the charging of petroleum naphtha mixed phase generate hydrogen (H from hydrofining through steam reforming reaction
2), methane (CH
4), carbon monoxide (CO), carbonic acid gas (CO
2) method.It is characterized in that: refinery's thousand gas remove wherein hydrogen sulfide (H through diethanolamine
2S), carbon monoxide (CO), carbonic acid gas (CO
2) after, after compressed the boosting of thousand gas of the refinery behind gas-liquid separation, the separatory, with the charging of petroleum naphtha mixed phase, through hydrofining, desulfurization, deep refining, make the hydrocarbon flow behind the mixed phase become the steam reforming charging, generate hydrogen, methane, carbon monoxide, carbonic acid gas through conversion reaction.
2, method according to claim 1 is characterized in that: the ratio that the amount of oil refinery dry gas accounts for whole mixed phase charging is can regulate arbitrarily in 20～80%(wt) scopes.
3, method according to claim 1, it is characterized in that: in the hydrofining operation, utilize in the oil refinery dry gas contained 18～30%(V) hydrogen, its Alkene hydrogenation of contained 10～20%(V) is saturated to＜1%(V), carbonylsulfide (COS), mercaptan (RSH) change into hydrogen sulfide (H
2S).Its processing condition are:
Reaction pressure: 1.0～4.5MPa
Temperature of reaction: 180～380 ℃
Oil refinery dry gas gas air speed: 500～3000h
-1
Petroleum naphtha liquid air speed: 0.5～4.0h
-1
Hydrogen/rare mol ratio:＞1.10
Charging sulfur-bearing: ≮ 3ppm
4, method according to claim 1 is characterized in that: in the desulfurization process, adopt zinc oxide (ZnO) desulfurization, make total sulfur＜0.5ppm.Its processing condition are:
Reaction stagnation pressure: 1.0～4.5MPa
Temperature of reaction: 250～400 ℃
Oil refinery dry gas gas air speed: 500～3000h
-1
Petroleum naphtha liquid air speed: 0.5～2.0h
-1
5, method according to claim 1 is characterized in that: in the deep refining operation, the sulphur in the hydrocarbon flow, chlorine, arsenic can be taken off the level to ppb; Alkene takes off the level to ppm; Aromatic hydrocarbons in the petroleum naphtha by 10～20%(wt) reduce to＜1%(wt).Its processing condition are:
Reaction stagnation pressure: 1.0～4.5MPa
Temperature of reaction: 140～240 ℃
Oil refinery dry gas gas air speed: 500～3000h
-1
Petroleum naphtha liquid air speed: 0.5～2.0h
-1
6, method according to claim 1 is characterized in that: in the hydrofining operation, the catalyzer that uses is cobalt-molybdenum, nickel-molybdenum, nickel-molybdenum-tungsten or the cobalt-molybdenum-nickel Hydrobon catalyst as active ingredient, first-selected CH-6,481-3 catalyzer.
7, method according to claim 1 is characterized in that: in the hydrofining operation, petroleum naphtha adopts the low highly active state of recycle ratio of low temperature to operate as heat-absorbing medium.
8, method according to claim 1 is characterized in that: in the deep refining operation, select high-nickel catalyst for use, first-selected 0501 catalyzer.
9, method according to claim 1, it is characterized in that: in the steam reforming operation, owing to removed the objectionable impurities that easily makes conversion catalyst poisoning, carbon distribution effectively through removing sour gas, hydrofining, desulfurization and deep refining operation, can make conversion reaction under the state of low temperature high activity, generate hydrogen, methane, carbon monoxide, carbonic acid gas.
10, according to claim 1 or 9 described methods, it is characterized in that: in the steam reforming operation, steam reforming catalysts can be selected from RKNR and Z409/Z405.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92111165 CN1055108C (en) | 1992-10-27 | 1992-10-27 | Preparation of hydrogen, methane, carbon monoxide, carbon dioxide by self-hydrogenation refining and mixed phase feeding of dry gas and naphtha from refining plant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92111165 CN1055108C (en) | 1992-10-27 | 1992-10-27 | Preparation of hydrogen, methane, carbon monoxide, carbon dioxide by self-hydrogenation refining and mixed phase feeding of dry gas and naphtha from refining plant |
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| Publication Number | Publication Date |
|---|---|
| CN1075740A true CN1075740A (en) | 1993-09-01 |
| CN1055108C CN1055108C (en) | 2000-08-02 |
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|---|---|---|---|
| CN 92111165 Expired - Fee Related CN1055108C (en) | 1992-10-27 | 1992-10-27 | Preparation of hydrogen, methane, carbon monoxide, carbon dioxide by self-hydrogenation refining and mixed phase feeding of dry gas and naphtha from refining plant |
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| CN1037853C (en) * | 1995-08-31 | 1998-03-25 | 中国石化北京设计院 | Method for producing raw material of synthetic gas from rich tail gas of coking plant |
| CN1049873C (en) * | 1996-10-21 | 2000-03-01 | 中国石化茂名石油化工公司 | Technology for preparing hydrogen by mixing dry gas and light oil of refinery |
| CN102090968A (en) * | 2011-01-28 | 2011-06-15 | 武汉耦合医学科技有限责任公司 | Flushing-free medical care product for heads and preparation method thereof |
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| CN1037853C (en) * | 1995-08-31 | 1998-03-25 | 中国石化北京设计院 | Method for producing raw material of synthetic gas from rich tail gas of coking plant |
| CN1049873C (en) * | 1996-10-21 | 2000-03-01 | 中国石化茂名石油化工公司 | Technology for preparing hydrogen by mixing dry gas and light oil of refinery |
| CN102090968A (en) * | 2011-01-28 | 2011-06-15 | 武汉耦合医学科技有限责任公司 | Flushing-free medical care product for heads and preparation method thereof |
| CN103508418A (en) * | 2012-06-18 | 2014-01-15 | 中国石油化工集团公司 | Start gas heating system in process of hydrogen production from water vapor and heating method |
| CN103508418B (en) * | 2012-06-18 | 2015-08-12 | 中国石油化工集团公司 | Go into operation gas heating system and heating means in water vapour process for making hydrogen |
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| CN106753558A (en) * | 2015-11-20 | 2017-05-31 | 中国石油化工股份有限公司 | The method of dry gas producing ethylene cracking material through hydrogenation |
| CN106753560A (en) * | 2015-11-20 | 2017-05-31 | 中国石油化工股份有限公司 | A kind of technique of dry gas preparing ethylene cracking material by hydrogenation |
| CN106753560B (en) * | 2015-11-20 | 2019-01-25 | 中国石油化工股份有限公司 | A kind of technique of dry gas preparing ethylene cracking material by hydrogenation |
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