CN100529022C - Triphase slurry bed reactor for preparing liquid fuel with synthetic gas - Google Patents
Triphase slurry bed reactor for preparing liquid fuel with synthetic gas Download PDFInfo
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- CN100529022C CN100529022C CNB2007100379605A CN200710037960A CN100529022C CN 100529022 C CN100529022 C CN 100529022C CN B2007100379605 A CNB2007100379605 A CN B2007100379605A CN 200710037960 A CN200710037960 A CN 200710037960A CN 100529022 C CN100529022 C CN 100529022C
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Abstract
The triphase slurry bed reactor for preparing liquid fuel with synthetic gas includes one cylindrical reaction section and one cylindrical separating section over the reaction section with diameter ratio of 1 to 1.5-1.2 and height ratio of 1 to 0.2-0.5; one heat exchange member inside the reaction section, one gas distributor connected to the gas inlet of the reaction section, one liquid phase material inlet in the reaction section or the separating section, one liquid product outlet in the reaction section and one gas outlet in the top of the separating section. The triphase slurry bed reactor has the capacity of maintaining the activity of catalyst for long time use, simple structure, low manufacture cost and easy operation.
Description
Technical field
The present invention relates to a kind of slurry bed reactor, be specifically related to can be back to back the mutually triphase slurry bed reactor of oil product of a kind of gas-liquid, also give simultaneously and be applied to other field.
Background technology
The maximization of production equipments such as, dme synthetic along with F-T and alcohol-ether fuel, three-phase (gas-liquid-solid) slurry bed reactor has obtained unprecedented development.Though have a lot of documents and patent to propose the pattern of various triphase slurry bed reactor, CN 1233451C), " reactor for chemical reactions in triphasic system " (Granted publication number: CN 1174799C) etc., all there is problem miscellaneous in above-mentioned reactor as " a kind of gas-liquid-solid three-phase of operate continuously slurry attitude bed industrial reactor " (Granted publication number:.
Conclusion is got up, and there is following problem in present triphase slurry bed reactor:
(1) there is tangible scale-up problem in the mechanical stirring tank reactor, can only be used for the laboratory reaction device;
(2) circulating, jetting type or spouted hearth reactor are easy to cause the wearing and tearing of catalyzer simultaneously because the problem of flow pattern is unfavorable to the catalyst activity that is present in the liquid phase;
(3) general air-flow bubbling suspension reactor, liquid-solid suspension is discharged reactor and is handled outward, not only causes the catalyst recovery difficulty, and very easily causes catalyst deactivation;
(4) the gas-liquid-solid three-phase paste state bed reactor of built-in heat exchanger and liquid-solid separation device, the reactor internal components complexity, the manufacturing expense height, operation easier is big.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of triphase slurry bed reactor, to overcome the above-mentioned defective that prior art exists.
The triphase slurry bed reactor that the present invention proposes comprises:
Conversion zone with cylindrical shell;
Be arranged on the segregation section that said conversion zone top is connected with conversion zone with cylindrical shell;
The diameter of segregation section and the diameter ratio of conversion zone are 1.5～1.2: 1, and the ratio of height is 0.2～0.5: 1, and its objective is in order to ensure reacted gas partly has enough spaces to realize separating with the most granules of catalyst carried secretly and part mist;
Be arranged on the heat exchange component in the said conversion zone, the import of heat exchange component is arranged on the housing of conversion zone with outlet;
Be arranged on the gas distributor that is connected with the gas inlet of conversion zone bottom;
Be arranged on the liquid phase inlet on the cylindrical shell of conversion zone or segregation section;
Be arranged on the liquid-phase product outlet on the conversion zone cylindrical shell, be used to draw liquid phase substance;
Be arranged on the pneumatic outlet at segregation section top.
The said triphase slurry bed reactor of the present invention, can be used for gas-liquid-solid triphasic chemical reaction, liquid phase wherein can be an inert heat carrier, also can be raw material or reaction product, building-up reactions can be carried out under 120 ℃～400 ℃ of temperature, pressure 1.0MPa～10.0Mpa, reaction can be that thermopositive reaction can be thermo-negative reaction also, is particularly suitable for that picture F-T is synthetic, dme etc. is by synthetic gas preparing liquid fuel process and other similar procedure of gas-liquid-solid three-phase reaction system.
Triphase slurry bed reactor of the present invention keeps activity of such catalysts easily, and the wearing and tearing of catalyzer are little, and catalyzer can recycle for a long time, is difficult for causing catalyst deactivation, and reactor internal components is simple, and manufacturing expense is low, processing ease.
Description of drawings
Fig. 1 is a triphase slurry bed reactor structural representation of the present invention.
Fig. 2 is the gas distributor structural representation.
Embodiment
Referring to Fig. 1, the triphase slurry bed reactor that the present invention proposes comprises:
Conversion zone 8 with cylindrical shell;
Be arranged on the segregation section with cylindrical shell 2 that said conversion zone top is connected with conversion zone 8;
The diameter ratio of the diameter of segregation section 2 and conversion zone 8 is 1.5～1.2: 1, and the ratio of height is 0.2～0.5: 1, and its objective is in order to ensure reacted gas partly has enough spaces to realize separating with the most granules of catalyst carried secretly and part mist;
Be arranged on the heat exchange component 7 in the said conversion zone 8, the import of heat exchange component 7 is arranged on the housing of conversion zone with outlet;
Be arranged on the gas distributor 9 that is connected with gas inlet 4 of conversion zone 8 bottoms;
Be arranged on the liquid phase inlet 6 on the cylindrical shell of conversion zone 8 or segregation section 2;
Be arranged on the liquid-phase product outlet 10 on conversion zone 8 cylindrical shells;
Be arranged on the pneumatic outlet 1 at segregation section 2 tops;
Referring to Fig. 2, said gas distributor 9 comprises the gas inlet pipe 91 that is connected with gas inlet 4, the distribution pipe 3 that is provided with aperture 5 that is connected with gas inlet pipe 91, the percentage of open area of 3 aperture 5 is 1 ‰～10 ‰ on the distribution pipe, direction down, axially become 40～50 degree angles with reactor, the diameter of aperture 5 is 0.5～1.5mm;
Can triphase slurry bed reactor the most important factor of industrial application be exactly to select suitable gas distributor, and the key of suitable gas distributor is exactly correct percentage of open area, opening diameter and angle, the working rate that the present invention chooses, opening diameter and angle prove safe and reliable through the check of secular experimental verification and industrial demonstration unit actual motion.
Said heat exchange component 7 is the variable density spiral pipe, the contriver finds, slurry forms the trend that density reduces gradually mutually vertically from bottom to top, lower catalytic agent density is big, the lower gas reactant concn is big simultaneously, therefore it is more violent to be reflected at the bottom, and thermopositive reaction forms more reaction heat, and thermo-negative reaction needs more heat; And the top density of catalyst is little, and the upper gas reactant concn is little simultaneously, and it is more steady therefore to be reflected at the bottom, and thermopositive reaction forms less reaction heat, and thermo-negative reaction needs less heat.At above-mentioned phenomenon, the present invention adopts variable density helical disk tubular type interchanger, said interchanger heat interchanging area increases to the bottom gradually from reactor top vertically, in y=(1.2～2.5) x ratio, wherein x is a reactor equivalent length vertically, and y is an interchanger equivalent heat exchange density vertically;
It is 1 measure unit that term " equivalent length " refers to from the interchanger top, the downward length and the ratio of this gauge length from the interchanger top, equivalent heat exchange density=from the heat interchanging area at interchanger top is 1 measure unit, the downward heat interchanging area and the ratio of this measure unit from the interchanger top.
Further, conversion zone 8 cylindrical shells are provided with a plurality of liquid-phase product outlets 10 from top to down, because if having a plurality of liquid-phase products, then different liquid-phase products has different density, need be in the different position discharging of phase reactor;
Further, export 10 places at liquid-phase product and be provided with the silk screen of aperture, flow out to stop catalyzer less than catalyzer;
Further, scum dredger is set, is used to remove most of liquid phase medium at segregation section 2 tops.
Embodiment 1
Adopt the triphase slurry bed reactor of Fig. 1 and the gas distributor of Fig. 2.
Wherein: the reactor reaction section diameter is 1.45 meters, highly be 22 meters, the separate part diameter is 1.8 meters, highly be 6 meters, the gas distributor percentage of open area is 8 ‰, and the perforate direction axially becomes miter angle with reactor down, hole diameter is 1.0mm, y=1.2x, wherein x is a reactor equivalent length vertically, y is an interchanger equivalent heat exchange density vertically;
With the synthetic gas is raw material, and single stage method is produced 30000 tons of alcohol-ether fuels per year, and the average gas holdup of this reactor is 0.189,12.38 tons of catalyst qualities, and inertia liquid phase thermal barrier quality is 23 tons.In the synthetic gas, CO content is 28%, and H2 is 68%, and CO2 is 3% (volume), is 250 ℃ in temperature, and when pressure was 5.0Mpa, the CO transformation efficiency was 0.6667, and the dme annual production is 27626.67 tons, and the methyl alcohol annual production is 3746.59 tons.
Catalyzer adopts commercial Cu-Zn-Al methanol synthesis catalyst XNC-98 (Southwest Chemical Research and Design Institute production) and CM-3-1 molecular sieve methanol dehydration catalyst (Southwest Chemical Research and Design Institute production);
Inertia liquid phase thermal barrier is a medical liquid paraffin oil.
Embodiment 2
Adopt the triphase slurry bed reactor of Fig. 1 and the gas distributor of Fig. 2.
Wherein:
The reactor reaction section diameter is 3.25 meters, highly be 23 meters, the separate part diameter is 3.9 meters, highly be 7 meters, the gas distributor percentage of open area is 8 ‰, and the perforate direction axially becomes miter angle with reactor down, hole diameter is 1mm, y=2.5x, wherein x is a reactor equivalent length vertically, y is an interchanger equivalent heat exchange density vertically;
With the synthetic gas is raw material, and single stage method is produced 300000 tons of alcohol-ether fuels per year, and the average gas holdup of this reactor is 0.189,120 tons of catalyst qualities, and inertia liquid phase thermal barrier quality is 230 tons.CO content is 28% in the synthetic gas, H
2Be 68%, CO
2Being 3% (volume), is 250 ℃ in temperature, and when pressure was 5.0Mpa, the CO transformation efficiency was 0.67, and the dme annual production is 280000 tons, and the methyl alcohol annual production is 36000 tons.
Catalyzer adopts commercial Cu-Zn-Al methanol synthesis catalyst XNC-98 (Southwest Chemical Research and Design Institute production) and CM-3-1 molecular sieve methanol dehydration catalyst (Southwest Chemical Research and Design Institute production);
Inertia liquid phase thermal barrier is a medical liquid paraffin oil.
Adopt the triphase slurry bed reactor of Fig. 1 and the gas distributor of Fig. 2.
Wherein: the reactor reaction section diameter is 1.45 meters, highly be 22 meters, the separate part diameter is 1.8 meters, highly be 6 meters, the gas distributor percentage of open area is 8 ‰, and the perforate direction axially becomes 50 degree angles with reactor down, hole diameter is 1mm, y=2.0x, wherein x is a reactor equivalent length vertically, y is an interchanger equivalent heat exchange density vertically;
With the synthetic gas is raw material, synthetic 30,000 tons of heavy hydrocarbon fuel, the H in the synthetic gas of producing per year of F-T
2/ CO is 2.0, is 220 ℃ in temperature, and when pressure was 2.5Mpa, the CO transformation efficiency reached 84.88%, and the selectivity of hydrocarbon, CH4 and CO2 is respectively 99.63%, 5.47% and 0.37%, and the selectivity of heavy hydrocarbon is 88.16%.
Catalyzer adopts homemade F-T synthetic catalyst, and the preparation method is as follows:
Catalyzer adopts profit immersion process for preparing just, drips the Zr (NO of concentration known according to the water regain of carrier
3)
45H
2The O aqueous solution, Co (NO is flooded in dipping, dry, roasting then
3)
26H
2O and RuCl
3Mixed aqueous solution, obtain ZrO
2Modification Co-Ru/ γ-Al
2O
3Catalyzer (hereinafter to be referred as catalyzer) the wherein massfraction of each component is 15.15%Co0.38%Ru8.71%ZrO
2/ γ-Al
2O
3
Inertia liquid phase thermal barrier is the liquid phase oil product.
Claims (5)
1. a triphase slurry bed reactor that is used for by the synthetic gas preparing liquid fuel is characterized in that, comprising:
Conversion zone (8) with cylindrical shell;
Be arranged on the segregation section with cylindrical shell (2) that said conversion zone top is connected with conversion zone (8), the diameter ratio of the diameter of segregation section (2) and conversion zone (8) is 1.5～1.2: 1, and the ratio of height is 0.2～0.5: 1;
Be arranged on the heat exchange component (7) in the said conversion zone (8), the import of heat exchange component (7) is arranged on the housing of conversion zone with outlet;
Be arranged on the gas distributor (9) that is connected with gas inlet (4) of conversion zone (8) bottom;
Be arranged on the liquid phase inlet (6) on the cylindrical shell of conversion zone (8) or segregation section (2);
Be arranged on the liquid-phase product outlet (10) on conversion zone (8) cylindrical shell;
Be arranged on the pneumatic outlet (1) at segregation section (2) top;
Said gas distributor (9) comprises the gas inlet pipe (91) that is connected with gas inlet (4), the distribution pipe (3) that is provided with aperture (5) that is connected with gas inlet pipe (91), the percentage of open area of the aperture (5) on the distribution pipe (3) is 1 ‰～10 ‰, direction down, axially become 40～50 degree angles with reactor, the diameter of aperture (5) is 0.5～1.5mm.
2. the triphase slurry bed reactor that is used for by the synthetic gas preparing liquid fuel according to claim 1 is characterized in that, said heat exchange component (7) is the variable density spiral pipe.
3. the triphase slurry bed reactor that is used for by the synthetic gas preparing liquid fuel according to claim 1 is characterized in that, conversion zone (8) cylindrical shell is provided with a plurality of liquid-phase product outlets (10) from top to down.
4. the triphase slurry bed reactor that is used for by the synthetic gas preparing liquid fuel according to claim 3 is characterized in that, locates to be provided with the silk screen of aperture less than catalyzer in liquid-phase product outlet (10).
5. the triphase slurry bed reactor that is used for by the synthetic gas preparing liquid fuel according to claim 1 is characterized in that, segregation section (2) top is provided with scum dredger.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100379605A CN100529022C (en) | 2007-03-09 | 2007-03-09 | Triphase slurry bed reactor for preparing liquid fuel with synthetic gas |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2007100379605A CN100529022C (en) | 2007-03-09 | 2007-03-09 | Triphase slurry bed reactor for preparing liquid fuel with synthetic gas |
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| CN101020839A CN101020839A (en) | 2007-08-22 |
| CN100529022C true CN100529022C (en) | 2009-08-19 |
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| CN102921355B (en) * | 2011-08-08 | 2016-03-30 | 中国石油化工股份有限公司 | A kind of calandria type fixed bed reactor and coal bed gas deoxidation method |
| CN105617959A (en) * | 2016-01-15 | 2016-06-01 | 湖南弘润化工科技有限公司 | Reaction device for continuously producing benzoic acid by virtue of toluene liquid-phase air oxidation method |
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Non-Patent Citations (2)
| Title |
|---|
| 含氮合成气在三相淤浆床- 固定床中直接合成二甲醚. 刘宏伟，聂兆广，刘殿华，应卫勇，房鼎业.燃料化学学报，第VOL.33卷第NO.3期. 2005 |
| 含氮合成气在三相淤浆床- 固定床中直接合成二甲醚. 刘宏伟，聂兆广，刘殿华，应卫勇，房鼎业.燃料化学学报，第VOL.33卷第NO.3期. 2005 * |
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