CN1055108C - Preparation of hydrogen, methane, carbon monoxide, carbon dioxide by self-hydrogenation refining and mixed phase feeding of dry gas and naphtha from refining plant - Google Patents
Preparation of hydrogen, methane, carbon monoxide, carbon dioxide by self-hydrogenation refining and mixed phase feeding of dry gas and naphtha from refining plant Download PDFInfo
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- CN1055108C CN1055108C CN 92111165 CN92111165A CN1055108C CN 1055108 C CN1055108 C CN 1055108C CN 92111165 CN92111165 CN 92111165 CN 92111165 A CN92111165 A CN 92111165A CN 1055108 C CN1055108 C CN 1055108C
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Abstract
The present invention relates to a method for the development and the utilization of refinery gas as a byproduct in an oil refinery. The method comprises the following steps: eliminating hydrogen sulphide, carbon monoxide and carbon dioxide in the refinery gas by 2-ethanolamine; carrying out gas-liquid separation for the refinery gas; carrying out pressure boost and compression for the refinery gas after the liquid is separated; mixing the refinery gas with naphtha for feeding; arbitrarily regulating the refinery gas within the range of 20 to 80 wt% of the mixed-phase feeding; converting oil airflow with the phase mixing into good vapor conversion feeding by hydrofining, desulfurization and deep refining; generating hydrogen gas, methane, the carbon monoxide and the carbon dioxide by a conversion reaction. Thereby, the present invention provides an economic and effective method for further producing synthetic ammonia, methanol, vapour, the hydrogen gas, 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 main component 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, hydrogenation of olefins 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 alkane in the hydrocarbon gas and alkene 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 reforming 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% (hydrogenation of olefins v) is saturated to＜and 1% (v), COS, RSH etc. change 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, aromatic hydrocarbons in the petroleum naphtha can be reduced to＜1% (wt) by 10～20% (wt), the alkene in the oil refinery dry gas is reduced to the ppm level, and 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 (unstripped gas and hot hydrocarbon flow heat exchange heating process, reactant and cold conditions hydrocarbon flow heat exchange cooling process), (7) hydrofining operation, (8) zinc oxide desulfurization operation, (9) deep refining operation, (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 the hydrogen/alkene 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 Hydrobon catalyst in the device), (hydrogenation of olefins v) is saturated, makes total olefin＜1% (v) with 10～20% in the oil refinery dry gas, 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 is the catalyst for refining of active ingredient with nickel in the device), can be with detrimental impurity sulphur wherein, chlorine, arsenic etc. take off the level to ppb, alkene in the oil refinery dry gas is reduced to the ppm level, aromatic hydrocarbons in the petroleum naphtha is reduced to＜1% (wt) by 10～20% (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 matter of utmost importance in the conversion process operation.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 before advancing the steam reforming stove oil refinery dry gas＜1% (v), could satisfy the requirement of steam reforming charging.For this reason, the present invention utilizes that contained 18～30% in the oil refinery dry gas (contained 10～20% (hydrogenation of olefins v) is saturated with it for hydrogen v) (from hydrogenation).
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) scope 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
The charging sulphur content, ≮ 3ppm
Catalyzer is the Hydrobon catalyst of active ingredient with cobalt-molybdenum, nickel-molybdenum or nickel-molybdenum-tungsten, and its carrier is an aluminum oxide, or aluminum oxide interpolation silicon-dioxide, or aluminum oxide adds titanium dioxide.The model of domestic Hunan Chang Ling general petrochemicals factory catalyst plant production is that the catalyzer of CH-6 and the model of Wenzhou, Zhejiang catalyst plant production are the catalyzer of 481-3, all is well behaved Hydrobon catalyst.
The hydrocarbon steam conversion method is to be the most economical method of the production synthetic ammonia or the hydrogen of raw material with hydrocarbon gas and petroleum naphtha.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 to be active ingredient with nickel, is carrier with aluminum oxide interpolation magnesium oxide, calcium oxide.In conversion reaction, the 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, HCl, and generate NiS, NiCl with nickel reactant in the catalyzer
2, cause 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 the level to ppm, aromatic hydrocarbons takes 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) are
The reaction stagnation pressure, 1.0～4.5MPa
Temperature of reaction, 250～400 ℃
The gas air speed, 500～3000h
-1
Petroleum naphtha liquid air speed, 0.5～2.0h
-1
Desulfurization catalyst, zinc oxide.The model of domestic southization group company's catalyst plant and the Fine Chemical Works production of Kunshan, Jiangsu is T305, T306 Zinc oxide catalytic, is good desulfurization catalyst.
The processing condition of deep refining reactor of the present invention (8) are
Reaction 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
The deep refining catalyzer is active ingredient with nickel, and its carrier is aluminum oxide or diatomite.The model of domestic southization group company catalyst plant production is the catalyzer of 0501 (existing model is NCG), is a kind of good deep refining 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
Steam reforming catalysts is active ingredient with nickel, adds magnesium oxide with aluminum oxide, and calcium oxide etc. are carrier.The model of domestic Liaohe River catalyst plant production is that the model of Z403H (model that is similar to the rope production of Denmark Top is RKNR) and the catalyst plant production of Qilu Petrochemical company is the steam reforming catalysts of Z405/Z409, all is well behaved steam reforming catalysts.
The present invention compared with prior art has following advantage:
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, material sulphur, chlorine, the arsenic of easy poisoning carbon distribution in the steam reforming reaction can be taken off the level to ppb, alkene takes off the level to ppm, and aromatic hydrocarbons takes 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: (v) expression, represent with % (wt) by liquid or gas-liquid mixture with % for gas.Table 1:
Annotate: table 1 is formed for the oil refinery dry gas that removes behind the sour gas
| Component | ％(V) |
| | 18～30 |
| | 5～8 |
| CH 4 | 35～45 |
| C 2H 4 | 6～10 |
| C 2H 6 | 8～10 |
| C 3H 6 | 8～10 |
| C 3H 8 | 2～4 |
| i-C 4H 10 | 1～3 |
| n 1i-C 4H 8 | 1～2 |
| n-C 4H 8 | ＜1 |
| Instead-butene-2 | ＜1 |
| Suitable-butene-2 | ＜1 |
| Divinyl | ＜0.5 |
| C 6 | ＜1 |
| CO | ＜1 |
| CO 2 | ＜1 |
| H 2S+COS | ＜0.02 |
| H 2O | ＜1 |
Claims (1)
1. hydrogen is produced in oil refinery dry gas and the charging of petroleum naphtha mixed phase, methane, carbon monoxide, the method of carbonic acid gas, oil refinery dry gas removes wherein hydrogen sulfide through diethanolamine, carbon monoxide, behind the carbonic acid gas, through gas-liquid separation, refinery gas behind the separatory is compressed boost after, 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 through conversion reaction, methane, carbon monoxide, carbonic acid gas, the blending ratio of oil refinery dry gas and petroleum naphtha can be regulated in 20～80% scopes, and the processing condition of each operation are as follows:
(1) hydrofining operation:
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
The charging sulphur content, ≮ 3ppm
Catalyzer is the Hydrobon catalyst of active ingredient with cobalt-molybdenum, nickel-molybdenum or nickel-molybdenum-tungsten;
(2) desulfurization process:
The reaction stagnation pressure, 1.0～4.5MPa
Temperature of reaction, 250～400 ℃
The gas air speed, 500～3000h
-1
Petroleum naphtha liquid air speed, 0.5～2.0h
-1
Catalyzer is the zinc oxide desulfurization catalyzer;
(3) deep refining operation:
The 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
Catalyzer is the catalyst for refining of active ingredient with nickel;
(4) steam reforming reaction operation:
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 is the steam reforming catalysts of active ingredient with nickel.
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 CN1075740A (en) | 1993-09-01 |
| CN1055108C true CN1055108C (en) | 2000-08-02 |
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| CN101113127B (en) * | 2006-07-26 | 2010-05-12 | 李莉 | Method for preparing menthol by using refinery gas as raw material |
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| 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 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101113127B (en) * | 2006-07-26 | 2010-05-12 | 李莉 | Method for preparing menthol by using refinery gas as raw material |
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| CN1075740A (en) | 1993-09-01 |
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