CN103865562A - Method for preparing gasoline from methanol - Google Patents
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- CN103865562A CN103865562A CN201410062654.7A CN201410062654A CN103865562A CN 103865562 A CN103865562 A CN 103865562A CN 201410062654 A CN201410062654 A CN 201410062654A CN 103865562 A CN103865562 A CN 103865562A
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Abstract
The invention relates to a method for preparing gasoline from methanol. The method comprises the following steps: feeding the methanol into a section of methanol conversion fixed bed reactor filled with a synthetic gasoline catalyst after preheating; feeding a section of mixed hydrocarbon product of the conversion product into an oil-water separator to separate after condensing, so as to obtain crude gasoline, water and a dry gas, wherein one part of dry gas is returned to the methanol conversion reactor to control temperature rise, one part of dry gas is discharged out of the reaction system to maintain the system pressure; obtaining a C5<+> gasoline component and a liquefied gas from the crude gasoline after separating by a debutanizer; obtaining 94# gasoline and C9<+> heavy aromatics from the C5<+> gasoline component after separating by a gasoline separation tower; feeding the liquefied gas into two sections of aromatization reactors to react after mixing with a certain amount of methanol; and refluxing two sections of hydrocarbon products of the reaction product and mixing with one section of mixed hydrocarbon product. By adopting the method disclosed by the invention, the methanol conversion reaction is compounded with the liquidized gas aromatization, so that the service cycle of the synthetic oil catalyst and the gasoline yield are improved, and a heat source does not need to be externally added.
Description
Technical field
The present invention relates to the technology of preparing of petrochemical technology field gasoline, relate in particular to a kind of method of preparing gasoline by methanol.
Background technology
Preparing gasoline by methanol technique, be called for short MTG(methanol to gasoline) be to be succeeded in developing by Mobil company, its main-process stream is first taking coal or Sweet natural gas as raw material production synthetic gas, recycling synthetic gas is produced methyl alcohol, is finally high-octane rating by thick methanol conversion, without sulphur, free from chloride high-quality gasoline.United States Patent (USP) 3998898,4076761,4044061,4404414, the Patents of the preparing gasoline by methanol technique of the 4523046th, Mobil company alerting bulletin, adopts two sections of conversion process of fixed bed, and wherein first paragraph is dimethyl ether by methanol dehydration, the mixture of methyl alcohol out of first paragraph, dme, water enters second segment fixed-bed reactor, under the effect of ZSM-5 catalyzer, generates gasoline.
Government Of New Zealand once utilized the technology of Mobil company to build up methyl alcohol treatment capacity in 1984 be the MTG device of 1,600,000 tons/year, synthetic gasoline throughput is 560,000 tons/year, and device successful operation is after 10 years, because International Crude Oil is lower, synthetic oil cost is high, and MTG unit is forced to stop work.Along with the continuous rising of crude oil price, technique for preparing gasoline by methanol becomes the focus of world attention again in recent years.The key of technique for preparing gasoline by methanol is the exploitation of catalyzer, and the catalyzer adopting in existing technique for preparing gasoline by methanol is mostly modification or unmodified ZSM-5 molecular sieve catalyzer.
The preparing gasoline by methanol catalyzer that US4402867 announces is the ZSM-5 molecular sieve catalyzer of amorphous silicon modification, and the sial amount of substance ratio of ZSM-5 molecular sieve is 12, and the charge capacity of amorphous silicon is at least 0.3%.The gasoline products that methyl alcohol obtains after transforming on the ZSM-5 of silicon modification composed as follows: the alkane of the alkene of 50-75%, the aromatic hydrocarbons of 15-30%, 20% left and right.ZSM-5 molecular sieve is after amorphous silicon modification, and the coking deactivation speed of catalyzer significantly reduces, thus the life cycle that has extended catalyzer.Although this catalyzer has good stability, the olefin(e) centent in gasoline products is higher.
US4579999 has announced a kind of methyl alcohol and has been converted into after two reactor the technology of gasoline component, and first methyl alcohol change into C in the fluidized-bed reactor that ZSM-5 molecular sieve catalyzer is housed
2-C
4alkene and C
5 +hydrocarbon component.After refrigerated separation, C
2-C
4olefin component enters in the second segment reactor that olefinic polymerization ZSM-5 catalyzer is housed reacts, and further changes into gasoline component.
CN1923770A has announced a kind of technique of preparing hydrocarbons produce from methanol by one-step method, the method adopts fixed-bed reactor, methyl alcohol on acid Si-Al zeolite molecular sieve catalyst through intermolecular or intramolecular dehydration, generate the intermediate products such as methylene radical or dme, these intermediate products are under acidic zeolite effect, further there is the reactions such as carbon chain growth, polymerization, cyclisation, hydrogen transference, finally generate C
1-C
12hydrocarbon products.
CN101775310A has announced a kind of method of producing gasoline by fluidized bed process methanol, the method adopts fluidized-bed reactor, methyl alcohol is under the ZSM-5 molecular sieve catalyst action containing zirconium or iron content, obtain hydro carbons blending ingredients, product is after gas-liquid separation, and light hydrocarbon gas is sent into fluidized-bed reactor and carried out lighter hydrocarbons circulation after overdraft.
Preparing gasoline by methanol catalyzer adopts ZSM-5 molecular sieve catalyzer, along with the acidity of carrying out catalyzer of reaction reduces gradually, causes yield of gasoline significantly to reduce, and liquefied gas output increases, and now needs catalyzer to regenerate to recover its activity.The single pass life of preparing gasoline by methanol catalyzer is 18-20 days at present, and catalyzer is frequently regenerated not only needs a large amount of energy consumptions also can reduce the entire life of catalyzer.If increase liquid gas aromatization reaction device after methanol conversion, liquefied gas by product is converted into taking aromatic hydrocarbons as main hydrocarbon component, can improve yield of gasoline, extend the one way life cycle of methanol conversion catalyst.But liquid gas aromatization reaction is thermo-negative reaction, and the temperature of liquid gas aromatization reaction will be higher than the temperature of reaction of methanol conversion, therefore needs external heat source that reaction heat is provided.
Summary of the invention
The object of this invention is to provide a kind of method of preparing gasoline by methanol, the method is undertaken compound by methanol conversion and liquefied gas through aromatization technology, one way life cycle and the gasoline total recovery of catalyzer are improved, and in two sections of aromatization reactors, methanol conversion and liquefied gas through aromatization are coupled, can save the external heat source of aromatization process needs, thereby reduce system energy consumption.
The present invention is a kind of method of preparing gasoline by methanol, it is characterized in that, comprises the steps:
(1) methyl alcohol, after preheating, enters in one section of methanol conversion that Synthetic gasoline catalyst is housed, and is converted into one section of hydrocarbon mixture product as leading taking isoparaffin and aromatic hydrocarbons;
(2) described one section of hydrocarbon mixture product, after condensation, enters water-and-oil separator and separates, and product separation is become to raw gasline, water and dry gas three parts;
(3) a part of dry gas returns to one section of methanol conversion as circulation gas and controls temperature rise after compressor compression, and the molar ratio of circulation gas and methyl alcohol is 2:1～15:1; Another part dry gas is discharged reaction system to maintain system pressure as the venting of speeding; Raw gasline, after debutanizing tower separates, obtains C
5 +gasoline component and liquefied gas;
(4) C
5 +gasoline component obtains 94 after gasoline separation tower separates
#gasoline and C
9 +heavy aromatics;
(5) methyl alcohol enters in two sections of aromatization reactors and reacts after mixing with the ratio of described liquefied gas taking mass ratio as 0.5:1～5:1, the two-stage mixing hydrocarbon product obtaining refluxes and mixes with one section of hydrocarbon mixture product, as step 2) as described in after condenser condenses, enter water-and-oil separator and separate.
In the method for the preparing gasoline by methanol described in the invention described above, it is characterized in that, described in step 1), described Synthetic gasoline catalyst adopts the nano-ZSM-5 molecular sieve catalyzer of processing modification through NaOH, NaOH concentration is 0.05～1mol/L, treatment temp is 25～100 DEG C, and the treatment time is 0.5～12h; Working pressure in described one section of methanol conversion is 0.1～6.0MPa, and service temperature is 330～550 DEG C, and methanol quality air speed is 0.5～10h
-1;
Operation temperature in step 5) in two sections of aromatization reactors is 380～600 DEG C, pressure is 0.1～6.0MPa, catalyzer adopts the nano-ZSM-5 molecular sieve catalyzer of hydrothermal treatment consists and metal composite modification, hydrothermal treatment consists temperature is 400～800 DEG C, modified metal is one or more in Zn, Ni, La, Ga, Sn, Mg and Re, and content of metal is 1.0wt%～8.0wt%.
According to the method for preparing gasoline by methanol of the present invention, further preferred version comprises the steps:
(1) methyl alcohol, after preheating, enters in one section of methanol conversion that Synthetic gasoline catalyst is housed, and is 0.1～3.0MPa at working pressure, and service temperature is 360～420 DEG C, and methanol quality air speed is 0.5～3h
-1condition under, be converted into taking isoparaffin and aromatic hydrocarbons as one section of main hydrocarbon mixture product; Wherein synthetic oil catalyst adopts the nano-ZSM-5 molecular sieve catalyzer of processing modification through NaOH, and NaOH concentration is 0.1～0.6mol/L, and treatment temp is 60～90 DEG C, and the treatment time is 1～6h;
(2) taking isoparaffin and aromatic hydrocarbons as one section of main hydrocarbon mixture product is after condensation, enter water-and-oil separator and separate, product separation is become to raw gasline, water and dry gas three parts;
(3) a part of dry gas returns to one section of methanol conversion as circulation gas and controls temperature rise after compressor compression, and the molar ratio of circulation gas and methyl alcohol is 3:1～10:1; Another part dry gas is discharged reaction system as the venting of speeding and is maintained system pressure; Raw gasline, after debutanizing tower separates, obtains C
5 +gasoline component and liquefied gas;
(4) C
5 +gasoline component obtains 94 after gasoline separation tower separates
#gasoline and C
9 +heavy aromatics;
(5) methyl alcohol enters in two sections of aromatization reactors after mixing with the ratio of liquefied gas taking mass ratio as 0.5:1～3:1, is 420～480 DEG C in service temperature, under the condition that pressure is 0.1～3.0MPa, reacts, and obtains two-stage mixing hydrocarbon product.Aromatized catalyst adopts the nano-ZSM-5 molecular sieve catalyzer of hydrothermal treatment consists and metal composite modification, hydrothermal treatment consists temperature is 450～600 DEG C, modified metal is one or more in Zn, Ni, La, Ga, Sn, Mg and Re, and content of metal is 2.0wt%～6.0wt%;
(6) after described two-stage mixing hydrocarbon product mixes with described one section of hydrocarbon mixture product, if step (2) is after condenser condenses, enters water-and-oil separator and separate.
The principle of the inventive method is: methyl alcohol first, in one section of fixed-bed reactor, is converted into hydrocarbon mixture component under the effect of Synthetic gasoline catalyst, and after water-and-oil separator, product is divided into raw gasline, water and dry gas three parts.Raw gasline, after debutanizing tower, obtains C
5 +gasoline component and the liquefied gas that is rich in alkane.Liquefied gas with after a certain amount of methanol mixed, enter two sections of aromatization reactors that modified Nano ZSM-5 molecular sieve catalyzer is housed in react, product returns to water-and-oil separator.This technique is carried out the reaction of methanol conversion and liquefied gas through aromatization compound, can improve one way life cycle and the yield of gasoline of synthetic oil catalyst.In addition, the reaction of methanol conversion is strong exothermal reaction, and the liquid gas aromatization reaction that is rich in alkane is violent endothermic process, in two sections of aromatization reactors, by both couplings, can save the external heat source of aromatization process needs, thus reduction system energy consumption.By this technique, yield of gasoline (taking methanol quality as base) can reach 33～42%, and preferred version is 36～41%, and the one way life cycle of synthetic oil catalyst can reach 28～40 days, and preferred version is 30～35 days.
Compared with the method for existing preparing gasoline by methanol, the inventive method has following advantage:
1) methanol conversion and liquefied gas through aromatization technology are carried out compound, while causing yield of gasoline to decline when the activity decreased of synthetic oil catalyst, liquefied gas through aromatization can ensure higher yield of gasoline, therefore can extend the life cycle of synthetic oil catalyst; 2) in liquid gas aromatization reaction unit, utilize the heat release of methanol conversion to supplement the heat absorption of alkane aromatization, can reduce system energy consumption; 3) yield of gasoline and octane value are high, and yield of gasoline reaches as high as 42%, and owing to having more isoparaffin and aromatic hydrocarbons in gasoline products, gasoline octane rating (RON) can reach 94.
Brief description of the drawings
Fig. 1 is the process flow diagram of the method for preparing gasoline by methanol of the present invention.
In figure: 1-preheater; Mono-section of methanol conversion of 2-; 3-interchanger; 4-compressor; 5-water-and-oil separator; 6-debutanizing tower; Bis-sections of aromatization reactors of 7-; 8-gasoline separation tower.
Specific implementation method
In order to further illustrate preparing gasoline by methanol method provided by the invention, below in conjunction with drawings and the specific embodiments, the inventive method is described further.
As shown in Figure 1, methyl alcohol from raw material pipeline enters into one section of methanol conversion 2 after preheater 1 preheating, under synthetic oil catalyst effect, be converted into the hydrocarbon mixture component as leading taking isoparaffin and aromatic hydrocarbons, product enters water-and-oil separator 5 and separates after interchanger 3, product is divided into dry gas, raw gasline and water three parts, part dry gas returns to one section of methanol conversion 2 and controls temperature rise after compressor 4, the part dry gas discharge system of exitting as speeding.Raw gasline enters after debutanizing tower 6 separates and obtains liquefied gas and C
5 +gasoline, C
5 +gasoline obtains 94 after gasoline separation tower 8 separates
#gasoline and C
9 +heavy aromatics.Liquefied gas reacts in jointly entering two sections of aromatization reactors 7 with a certain amount of methyl alcohol, and reaction product enters water-and-oil separator 5 and separates after interchanger 3.
Embodiment 1
Synthetic oil catalyst in one section of methanol conversion fixed-bed reactor is the nano-ZSM-5 molecular sieve of processing through NaOH, and NaOH concentration is 0.1mol/L, and treatment temp is 60 DEG C, and the treatment time is 1h.One section of the reaction of methanol conversion condition: temperature of reaction is 360 DEG C, pressure is 0.5MPa, methanol quality air speed is 0.5h
-1, the mol ratio of circulation dry gas and methyl alcohol is 3:1.Two sections of methyl alcohol and liquefied gas through aromatization adopt the nano-ZSM-5 molecular sieve catalyzer of hydrothermal treatment consists and metal composite modification, and hydrothermal treatment consists temperature is 450 DEG C, then adopts equi-volume impregnating load Zn, Re, and wherein ZnO charge capacity is 2.0wt%, Re
2o
7charge capacity be 0.5wt%.Liquefied gas and aromatization of methanol reaction conditions: temperature of reaction is 420 DEG C, reaction pressure is 0.5MPa, methyl alcohol is 0.5:1 with liquefied gas quality ratio.Reaction result is in table 1.
Embodiment 2
Synthetic oil catalyst in one section of methanol conversion fixed-bed reactor is the nano-ZSM-5 molecular sieve of processing through NaOH, and NaOH concentration is 0.2mol/L, and treatment temp is 70 DEG C, and the treatment time is 3h.One section of the reaction of methanol conversion condition: temperature of reaction is 380 DEG C, pressure is 1.0MPa, methanol quality air speed is 2.0h
-1, the mol ratio of circulation dry gas and methyl alcohol is 5:1.Two sections of methyl alcohol and liquefied gas through aromatization adopt the nano-ZSM-5 molecular sieve catalyzer of hydrothermal treatment consists and metal composite modification, hydrothermal treatment consists temperature is 500 DEG C, then adopt equi-volume impregnating load Zn, Ni, wherein ZnO charge capacity is 2.0wt%, and the charge capacity of NiO is 2.0wt%.Liquefied gas and aromatization of methanol reaction conditions: temperature of reaction is 440 DEG C, reaction pressure is 1.0MPa, methyl alcohol is 1:1 with liquefied gas quality ratio.Reaction result is in table 1.
Embodiment 3
Synthetic oil catalyst in one section of methanol conversion fixed-bed reactor is the nano-ZSM-5 molecular sieve of processing through NaOH, and NaOH concentration is 0.4mol/L, and treatment temp is 80 DEG C, and the treatment time is 4h.One section of the reaction of methanol conversion condition: temperature of reaction is 380 DEG C, pressure is 2.0MPa, methanol quality air speed is 2.0h
-1, the mol ratio of circulation dry gas and methyl alcohol is 6:1.Two sections of methyl alcohol and liquefied gas through aromatization adopt the nano-ZSM-5 molecular sieve catalyzer of hydrothermal treatment consists and metal composite modification, and hydrothermal treatment consists temperature is 550 DEG C, then adopts equi-volume impregnating load Zn, Ga, Sn, and wherein ZnO charge capacity is 4.0wt%, Ga
2o
3charge capacity be 1.0wt%, SnO
2charge capacity be 0.5wt%.Liquefied gas and aromatization of methanol reaction conditions: temperature of reaction is 460 DEG C, reaction pressure is 2.0MPa, methyl alcohol is 2:1 with liquefied gas quality ratio.Reaction result is in table 1.
Embodiment 4
Synthetic oil catalyst in one section of methanol conversion fixed-bed reactor is the nano-ZSM-5 molecular sieve of processing through NaOH, and NaOH concentration is 0.6mol/L, and treatment temp is 85 DEG C, and the treatment time is 5h.One section of the reaction of methanol conversion condition: temperature of reaction is 420 DEG C, pressure is 3.0MPa, methanol quality air speed is 3.0h
-1, the mol ratio of circulation dry gas and methyl alcohol is 9:1.Two sections of methyl alcohol and liquefied gas through aromatization adopt the nano-ZSM-5 molecular sieve catalyzer of hydrothermal treatment consists and metal composite modification, and hydrothermal treatment consists temperature is 450 DEG C, then adopts equi-volume impregnating load Ni, La, and wherein NiO charge capacity is 4.0wt%, La
2o
3charge capacity be 2.0wt%.Liquefied gas and aromatization of methanol reaction conditions: temperature of reaction is 480 DEG C, reaction pressure is 3.0MPa, methyl alcohol is 3:1 with liquefied gas quality ratio.Reaction result is in table 1.
Table 1 embodiment 1～4 reaction result
Claims (3)
1. a method for preparing gasoline by methanol, is characterized in that, comprises the following steps:
1) methyl alcohol, after preheating, enters in one section of methanol conversion that Synthetic gasoline catalyst is housed, and is converted into one section of hydrocarbon mixture product as leading taking isoparaffin and aromatic hydrocarbons;
2) described one section of hydrocarbon mixture product, after condensation, enters water-and-oil separator and separates, and product separation is become to raw gasline, water and dry gas three parts;
3) a part of dry gas returns to one section of methanol conversion as circulation gas and controls temperature rise after compressor compression, and the molar ratio of circulation gas and methyl alcohol is 2:1～15:1; Another part dry gas is discharged reaction system to maintain system pressure as the venting of speeding; Raw gasline, after debutanizing tower separates, obtains C
5 +gasoline component and liquefied gas;
4) described C
5 +gasoline component obtains 94 after gasoline separation tower separates
#gasoline and C
9 +heavy aromatics;
5) methyl alcohol enters in two sections of aromatization reactors and reacts after mixing with the ratio of described liquefied gas taking mass ratio as 0.5:1～5:1, the two-stage mixing hydrocarbon product obtaining refluxes and mixes with one section of hydrocarbon mixture product, as step 2) as described in after condenser condenses, enter water-and-oil separator and separate.
2. method according to claim 1, it is characterized in that, described in step 1), described Synthetic gasoline catalyst adopts the nano-ZSM-5 molecular sieve catalyzer of processing modification through NaOH, and NaOH concentration is 0.05～1mol/L, treatment temp is 25～100 DEG C, and the treatment time is 0.5～12h; Working pressure in described one section of methanol conversion is 0.1～6.0MPa, and service temperature is 330～550 DEG C, and methanol quality air speed is 0.5～10h
-1;
Operation temperature in step 5) in two sections of aromatization reactors is 380～600 DEG C, pressure is 0.1～6.0MPa, catalyzer adopts the nano-ZSM-5 molecular sieve catalyzer of hydrothermal treatment consists and metal composite modification, hydrothermal treatment consists temperature is 400～800 DEG C, modified metal is one or more in Zn, Ni, La, Ga, Sn, Mg and Re, and content of metal is 1.0wt%～8.0wt%.
3. the method for preparing gasoline by methanol according to claim 2, is characterized in that, comprises the steps:
1) methyl alcohol, after preheating, enters in one section of methanol conversion that Synthetic gasoline catalyst is housed, and is 0.1～3.0MPa at working pressure, and service temperature is 360～420 DEG C, and methanol quality air speed is 0.5～3h
-1condition under, be converted into taking isoparaffin and aromatic hydrocarbons as one section of main hydrocarbon mixture product; Wherein synthetic oil catalyst adopts the nano-ZSM-5 molecular sieve catalyzer of processing modification through NaOH, and NaOH concentration is 0.1～0.6mol/L, and treatment temp is 60～90 DEG C, and the treatment time is 1～6h;
2) taking isoparaffin and aromatic hydrocarbons as one section of main hydrocarbon mixture product is after condensation, enter water-and-oil separator and separate, product separation is become to raw gasline, water and dry gas three parts;
3) a part of dry gas returns to one section of methanol conversion as circulation gas and controls temperature rise after compressor compression, and the molar ratio of circulation gas and methyl alcohol is 3:1～10:1; Part dry gas is discharged reaction system as the venting of speeding and is maintained system pressure; Raw gasline, after debutanizing tower separates, obtains C5
+gasoline component and liquefied gas;
4) described C5
+gasoline component obtains 94# gasoline and C9 after gasoline separation tower separates
+heavy aromatics;
5) methyl alcohol enters in two sections of aromatization reactors after mixing with the ratio of described liquefied gas taking mass ratio as 0.5:1～3:1, is 420～480 DEG C in service temperature, under the condition that pressure is 0.1～3.0MPa, reacts, and obtains two-stage mixing hydrocarbon product; The nano-ZSM-5 molecular sieve catalyzer of hydrothermal treatment consists and metal composite modification is housed in described aromatization reactor, hydrothermal treatment consists temperature is 450～600 DEG C, modified metal is one or more in Zn, Ni, La, Ga, Sn, Mg and Re, and content of metal is 2.0wt%～6.0wt%;
6) after described two-stage mixing hydrocarbon product mixes with described one section of hydrocarbon mixture product, as step 2) as described in after condenser condenses, enter water-and-oil separator and separate.
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| CN106669791A (en) * | 2017-01-20 | 2017-05-17 | 河北玺尧新能源科技有限公司 | Modified ZSM-5 molecular sieve catalyst and preparation method and application thereof |
| CN107162866A (en) * | 2017-04-19 | 2017-09-15 | 新地能源工程技术有限公司 | A kind of method and device of preparing gasoline by methanol coproduction dimethylbenzene |
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| CN110036094A (en) * | 2016-12-07 | 2019-07-19 | 埃克森美孚研究工程公司 | Comprehensive oxygenate conversion and olefin oligomerization |
| CN110760336A (en) * | 2019-09-17 | 2020-02-07 | 中国科学院青岛生物能源与过程研究所 | Method for directly preparing high-quality aviation oil from synthesis gas |
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