CN100512941C - Slurry bubble columun reactor having internal circulation and external heat-exchanging and the application - Google Patents
Slurry bubble columun reactor having internal circulation and external heat-exchanging and the application Download PDFInfo
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- CN100512941C CN100512941C CNB2007100370085A CN200710037008A CN100512941C CN 100512941 C CN100512941 C CN 100512941C CN B2007100370085 A CNB2007100370085 A CN B2007100370085A CN 200710037008 A CN200710037008 A CN 200710037008A CN 100512941 C CN100512941 C CN 100512941C
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- 239000002002 slurry Substances 0.000 title abstract description 23
- 239000003054 catalyst Substances 0.000 claims abstract description 36
- 239000012530 fluid Substances 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 9
- 239000000446 fuel Substances 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 96
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 230000015572 biosynthetic process Effects 0.000 claims description 11
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 11
- 238000003786 synthesis reaction Methods 0.000 claims description 9
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000007769 metal material Substances 0.000 claims description 2
- 239000002365 multiple layer Substances 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 239000007791 liquid phase Substances 0.000 claims 1
- 239000012071 phase Substances 0.000 claims 1
- 238000009826 distribution Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 21
- 238000005516 engineering process Methods 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 4
- 150000002430 hydrocarbons Chemical class 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- 210000000952 spleen Anatomy 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a slurry bed reactor with internal circulation and external heat exchange and its application. The slurry bed reactor comprises a tower-type Gas-Liquid-Solid three phase slurry bed reactor (12) with cylindrical casing, a tubular filter (11) arranged on the reactor (12), a sharp-crested orifice gas distributor, a heat exchanger (107), and a circulating pump (106), and can be used to generate gas or liquid fuel from synthetic gas in the presence of catalyst and liquid inert medium. In the invention, internal circulation of gas in the bottom of the reactor, on-line separation for catalyst inside the reactor, and carrying effect of fluid, form an internal circulation inside the reactor and a heat exchange outside the tower, thereby promoting axial even distribution of catalyst in the reactor and improving temperature distribution in tower, and the invention is provided with high space-time yield and low energy consumption, accordingly, mass production can be achieved easily.
Description
Technical field
The present invention relates to a kind of three phase slurry bed bioreactor, relating in particular to a kind of is raw material with the synthesis gas, the band gas interior circulation of preparation hydrocarbon and the three phase slurry bed bioreactor pattern of slurries external heat-exchanging.
Background technology
Said synthesis gas is produced by hydrocarbons such as coal, natural gas, oil, with H
2, CO, CO
2Be the main body component, all have been widely used in sectors of the national economy such as chemical industry, medical industry, light textile civilian industry and carriers.
Produce gas or liquid fuel by synthesis gas, in three phase slurry bed, carry out in the presence of catalyst usually, the reaction heat that produces is absorbed by inert liquid medium, thereby reaction can be carried out under isothermal.
The three phase slurry bed bioreactor obtains should having widely in chemical process.Many reports are arranged in existing literature and patent.A kind of gas-liquid-solid three-phase slurry attitude bed industrial reactor of continued operation is provided as Chinese patent 03151109.0; Gu Chinese patent 02808984.7 provides a kind of reactor that is used for gas/liquid or gas/liquid/reaction; Chinese patent 99127184.X provides a kind of circular tri-phase gas-liquid-solid reactor; South Africa Sasol company has made the paste state bed reactor skilled industryization, and the suitable efficient coal based synthetic gas that transforms of this technology, and the paste state bed reactor technology becomes artificial oil technology path of greatest concern at present.But the loadings of this slurry reactor catalyst has certain limit, so air speed can not be too big in the operation.
Simultaneously, the bottleneck problem of present three phase slurry bed also is the suspend separation problem of inhomogeneous and catalyst of solid.Because the catalyst suspension is measured when excessive in the paste state bed reactor, catalyst sedimentation and agglomeration can occur.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of slurry attitude bed reaction device and application thereof with interior circulation and external heat-exchanging, to overcome the above-mentioned defective that prior art exists.
The slurry attitude bed reaction device of circulation and external heat-exchanging in the said band of the present invention comprises:
Tower gas-liquid-solid three-phase paste state bed reactor with cylindrical shell;
Be vertically set on the tubular filter in the said reactor, said filter upper end closed,, body is a screen pack, the lower end is outlet;
Be arranged on the orifice gas distributor that the gas access with being arranged on reactor lower part in the said reactor is connected;
Be arranged on the gas products outlet of said reactor head;
Be arranged on the circulation fluid inlet on said reactor following side, orifice gas distributor top;
The heat exchanger that is connected by pipeline with said circulation fluid inlet;
With the circulating pump that said heat exchanger entrance is connected, the inlet of circulating pump exports with fluid product with the outlet of said filter bottom and is connected.
The slurry attitude bed reaction device of circulation and external heat-exchanging in the band of the present invention, can be used for synthesis gas based on hydrogen and carbon monoxide, in the presence of catalyst and liquid inert medium, reaction generates gas or liquid fuel, and said fuel comprises methyl alcohol, dimethyl ether, liquid hydrocarbon etc.
Inlet gas upwards enters reactor top by the orifice gas distributor, then with catalyst, under the carrying of inert media, adverse current upwards, while reaction solution fluid fuel, the inert media that contains catalyst filters by tubular filter, large granular catalyst is kept off outside tubular filter by tubular filter, after catalyst particle and inert media are delivered to the heat exchanger heating by circulating pump, enter paste state bed reactor once more by the circulation fluid inlet, can reduce the reactor bottom catalyst concentration effectively, improve reactor top catalyst concentration, thereby reach the effect that improves catalyst axial distribution inequality, effectively prevent catalyst sedimentation; If what generate is that fluid product is discharged by the fluid product outlet, be that gas products is then discharged by the gas products outlet as if what generate;
The catalyst particle and the inert media that come out from circulating pump cool off Returning reactors bottom, back through two heat exchanger heat exchange, promptly in the outside formation of reactor outer circulation, both can promote the solid suspension evenly, can remove reaction heat effectively again; Cooling medium can be water, gas or conduction oil.
Operating condition is: 220～280 ℃ of temperature, pressure 2.0～5.0Mpa, the reactor superficial gas velocity is 0.05～2.0m/s, gas holdup is 10%～80%, the catalyst grain size that is suitable for is 1～100 μ m, the mass percent concentration of catalyst in slurries is 1%～50%, and the orifice place of the orifice gas distributor speed of working off one's feeling vent one's spleen is 150～200m/s.The inert media recycle ratio is 5～20;
Said recycle ratio refers to the ratio of inert media total amount and internal circulating load in the reactor;
Compared with prior art, remarkable advantage of the present invention is: circulation in there is gas in reactor bottom, inside reactor are realized on-line separation for catalyst, and reactor top catalyst particle and inert media form the outer heat exchange of tower; Inside reactor is provided with the orifice gas distributor of controlling gas speed by resistance drop.The present invention utilizes the rolling action of fluid, heat exchange outside circulation and the tower in inside reactor and outside form respectively, it is circulation in gas forms in reactor, solid and catalyst particle be heat exchange Returning reactor bottom outside the outside formation of reactor, can prevent catalyst sedimentation effectively, promote catalyst to improve Temperature Distribution in the tower in that the reactor axial distribution is all even, the space time yield height, it is convenient to remove reaction heat, energy consumption is low, is easy to realize maximizing.
Description of drawings
Fig. 1 is the structural representation of the slurry attitude bed reaction device of circulation and external heat-exchanging in the band.
Fig. 2 is a star porous gas allocation member schematic diagram.
Fig. 3 is that the A-A of Fig. 2 is to view.
Fig. 4 is a grid-shaped porous gas allocation member schematic diagram.
The specific embodiment
Referring to Fig. 1, the slurry attitude bed reaction device of circulation and external heat-exchanging comprises in the band of the present invention:
Tower gas-liquid-solid three-phase paste state bed reactor 12 with cylindrical shell;
Be vertically set on the tubular filter 11 in the said reactor 12, said filter 11 upper end closeds, and be the arc or the taper shape of 15～75 ° of inclinations; Body is a screen pack, and the lower end is outlet;
Be arranged on orifice gas distributor 13 in the said reactor 12, that be connected with the gas access 103 that is arranged on reactor 12 bottoms;
Be arranged on the tail gas or the gas products outlet 104 at said reactor 12 tops;
Be arranged on the circulation fluid inlet 109 on said reactor 12 following sides, orifice gas distributor top;
The heat exchanger 107 that is connected by pipeline with said circulation fluid inlet 109;
With the circulating pump 106 that said heat exchanger 107 inlets are connected, the inlet of circulating pump 106 is connected with fluid product outlet 102 with the outlet 105 of said filter 11 bottoms;
Further, said reactor 12 is provided with cooling jacket 101, is used to remove the reaction liberated heat, the control reaction temperature;
Further, said reactor 12 from top to bottom is provided with a plurality of filters 11, and preferred 1～10, and be connected by pipeline with said circulating pump 106;
Further, referring to Fig. 2, said orifice gas distributor comprises:
Said gas inlet pipe 1 is connected with gas access 103, gas introduction tube 2 is arranged on the downside of gas inlet pipe 1, and be connected with gas inlet pipe 1, one end of wireway 4 is connected with porous gas allocation member 5, have a plurality of downward opening orifices 7 on the said porous gas allocation member 5, bump base plate 3 is arranged on the below of porous gas allocation member 5, inwall with sealing means and reactor fixes, cavity between bump base plate 3 and the porous gas allocation member 5 is bump chamber 8, cavity between bump base plate 3 and the gas inlet pipe 1 is gas buffer chamber 9, the other end of wireway 4 passes bump base plate 3, is connected with gas buffer chamber 9;
Inlet gas enters gas introduction tube 2 by gas inlet pipe 1, enter gas buffer chamber 9 then, enter porous gas allocation member 5 by wireway 4 again, be used for preliminary distribution to gas, by downward opening orifice 7, in bump chamber 8, finish the bump of gas,, upwards enter reactor 12 tops then to strengthen mass transfer;
Said porous gas allocation member 5 can adopt various ways, is provided with the grid-shaped that straight tube that star that straight tube that the endless tube of orifice 7, as shown in Figure 3 3～30 root bottom parts be provided with orifice 7 constitutes or bottom as shown in Figure 4 be provided with orifice 7 constitutes as the bottom;
The diameter of orifice 7 is 0.4～10mm, and percent opening is 0.01～2.0%; Preferably, reactor bottom is to the distance H of bump base plate 3
1Be 2～8 times of gas inlet pipe 1 diameter;
Preferably, bump base plate 3 is shaped as arc or circular arc, and radian is 120 °～150 °;
Preferably, the diameter ratio of the diameter of wireway 4 and gas inlet pipe 1 is 0.5～5;
Preferably, said filter is a kind of wide-aperture porous ceramics or metal material or multiple layer metal net.
Adopt the reactor of Fig. 1 and the orifice gas distributor of Fig. 2.
Three phase slurry bed bioreactor effective diameter is 3.2m, and effective depth 10m, the orifice diameter 10mm of orifice gas distributor, orifice work off one's feeling vent one's spleen speed for 180m/s, built-in 3 layers of filter,
The diameter of orifice 7 is 3mm, and percent opening is 0.33%;
Reactor bottom is to the distance H of bump base plate 3
1Be 200mm;
The diameter of wireway 4 is 80mm;
Said filter is that a kind of aperture is the wire netting of 0.01mm.
Synthesize example with the methyl alcohol of producing 300000 tons per year, unstripped gas is formed H
2=68%, CO=27%, CO
2=3%, CH
4+ N
2+ Ar=2%.Enter the pressure 5.0Mpa of the synthesis gas of three phase slurry bed bioreactor, 260 ℃ of temperature, superficial gas velocity 0.368m/s, flow 3.055 * 10
5Nm
3/ h; Catalyst concn 10% (kg/kg), as inert media, catalyst adopts the C307 type mesolow methanol synthesis catalyst of Research Institute of Nanjing Chemical Industry Group production with atoleine, and catalyst grain size is 50 μ m, and the inert media recycle ratio is 10;
Adopt the reactor of Fig. 1 and the orifice gas distributor of Fig. 4, synthesis gas is through the synthetic related hydrocarbons product that obtains of Fischer-Tropsch.
Three phase slurry bed bioreactor effective diameter is 3m, and effective depth 12m, the orifice diameter 2mm of orifice gas distributor, orifice work off one's feeling vent one's spleen speed for 150m/s, built-in 4 layers of filter,
The diameter of orifice (7) is 2mm, and percent opening is 0.13%; Reactor bottom is to the distance H of bump base plate (3)
1Be 150mm; Gas inlet pipe (1) diameter is 60mm; Reactor bottom is to the distance H of bump base plate (3)
1Be 150mm; Bump base plate (3) is shaped as arc, and radian is 150 °; The diameter of wireway (4) is 60mm; Said filter is that a kind of aperture is the wire netting of 0.001mm.Unstripped gas is formed CO/H
2=3/2, enter the pressure 2.5Mpa of the synthesis gas of three phase slurry bed bioreactor, 270 ℃ of temperature, air speed 10000h
-1, catalyst concn 10%Kg/Kg, as inert media, catalyst adopts Chinese patent 200410025515.3 disclosed copper auxiliary agent precipitated iron-based catalyst with atoleine, and catalyst grain size is 50 μ m, and the inert media recycle ratio is 6;
The synthetic evaluation index of Fischer-Tropsch mainly contains CO and H
2Conversion ratio, CH
4And CO
2Selectivity etc.The carbon monoxide conversion ratio is 91.3%, and hydrogen conversion is 66.5%, CH
4Selectivity is 14.1%, CO
2Selectivity is 29.6%.
Claims (10)
1. the paste state bed reactor of circulation and external heat-exchanging in the band is characterized in that, comprising:
Tower gas-liquid-solid three-phase paste state bed reactor (12) with cylindrical shell;
Be vertically set on the tubular filter (11) in the said reactor (12), said filter (11) upper end closed, body is a screen pack, the lower end is outlet;
Be arranged on the orifice gas distributor that the gas access (103) with being arranged on reactor (12) bottom in the said reactor (12) is connected;
Be arranged on the tail gas or the gaseous products outlet (104) at said reactor (12) top;
Be arranged on the circulation fluid inlet (109) on said reactor (12) following side, orifice gas distributor top;
The heat exchanger (107) that is connected by pipeline with said circulation fluid inlet (109);
With the circulating pump (106) that said heat exchanger (107) inlet is connected, the inlet of circulating pump (106) is connected with liquid-phase product outlet (102) with the outlet (105) of said filter (11) bottom.
2. the paste state bed reactor of circulation and external heat-exchanging is characterized in that said reactor (12) is provided with cooling jacket (101) in the band according to claim 1.
3. the paste state bed reactor of circulation and external heat-exchanging is characterized in that in the band according to claim 1, from top to bottom is provided with a plurality of filters (11) in the said reactor (12), and is connected by pipeline with said circulating pump (106).
4. the paste state bed reactor of circulation and external heat-exchanging in the band according to claim 1 is characterized in that said orifice gas distributor comprises:
Gas inlet pipe (1), gas introduction tube (2), wireway (4), porous gas allocation member (5) and bump base plate (3);
Said gas inlet pipe (1) is connected with gas access (103), gas introduction tube (2) is arranged on the downside of gas inlet pipe (1), and be connected with gas inlet pipe (1), one end of wireway (4) is connected with porous gas allocation member (5), have a plurality of downward opening orifices (7) on the said porous gas allocation member (5), bump base plate (3) is arranged on the below of porous gas allocation member (5), inwall with sealing means and reactor fixes, cavity between bump base plate (3) and the porous gas allocation member (5) is bump chamber (8), cavity between bump base plate (3) and the gas inlet pipe (1) is gas buffer chamber (9), the other end of wireway (4) passes bump base plate (3), is connected with gas buffer chamber (9).
5. the paste state bed reactor of circulation and external heat-exchanging in the band according to claim 4, it is characterized in that endless tube, 3～30 root bottom parts that said porous gas allocation member (5) is provided with orifice (7) for the bottom are provided with the grid-shaped that straight tube that star that the straight tube of orifice (7) constitutes or bottom be provided with orifice (7) constitutes.
6. the paste state bed reactor of circulation and external heat-exchanging is characterized in that the diameter of orifice (7) is 0.4～10mm in the band according to claim 5, and percent opening is 0.01～2.0%.
7. the paste state bed reactor of circulation and external heat-exchanging is characterized in that in the band according to claim 6, and reactor bottom is to the distance H of bump base plate (3)
1Be 2～8 times of gas inlet pipe (1) diameter, bump base plate (3) is shaped as arc or circular arc, and radian is 120 °～150 °, and the diameter ratio of the diameter of wireway (4) and gas inlet pipe (1) is 0.5～5.
8. the paste state bed reactor of circulation and external heat-exchanging is characterized in that said filter is a kind of wide-aperture porous ceramics or metal material or multiple layer metal net in the band according to claim 1.
9. according to the circulation and the paste state bed reactor of external heat-exchanging in claim 1 or the 3 described bands, it is characterized in that, said filter (11) upper end closed, and be the arc or the taper shape of 15～75 ° of inclinations.
10. according to the application of the circulation and the paste state bed reactor of external heat-exchanging in each described band of claim 1～8, it is characterized in that, be used for the synthesis gas based on hydrogen and carbon monoxide, in the presence of catalyst and liquid inert medium, reaction generates gas or liquid fuel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100370085A CN100512941C (en) | 2007-01-31 | 2007-01-31 | Slurry bubble columun reactor having internal circulation and external heat-exchanging and the application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100370085A CN100512941C (en) | 2007-01-31 | 2007-01-31 | Slurry bubble columun reactor having internal circulation and external heat-exchanging and the application |
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| Publication Number | Publication Date |
|---|---|
| CN101036865A CN101036865A (en) | 2007-09-19 |
| CN100512941C true CN100512941C (en) | 2009-07-15 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102872769A (en) * | 2012-09-28 | 2013-01-16 | 神华集团有限责任公司 | Gas distributor and slurry bed reactor and crude carbinol synthetic system both comprising same |
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| CN101721960B (en) * | 2008-10-29 | 2012-02-29 | 中国石油化工股份有限公司 | Fluidized bed reactor |
| CN102451651B (en) * | 2010-10-28 | 2014-12-31 | 中国石油化工股份有限公司 | Slurry bed loop reactor and application thereof |
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| CN103962067B (en) * | 2013-01-31 | 2017-02-08 | 中国科学院上海高等研究院 | Method for carrying out slurry bed reaction |
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| CN108905904B (en) * | 2018-09-05 | 2024-05-28 | 上海兖矿能源科技研发有限公司 | Gas distribution method for Fischer-Tropsch synthesis reactor |
| CN111921528A (en) * | 2020-06-28 | 2020-11-13 | 济南大学 | Method and system for preparing slurry bed Fischer-Tropsch synthesis catalyst slurry by pyrolyzing MOFs |
| CN113307271A (en) * | 2021-06-15 | 2021-08-27 | 新疆硅基新材料创新中心有限公司 | Tail gas emission structure and reduction furnace |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102872769A (en) * | 2012-09-28 | 2013-01-16 | 神华集团有限责任公司 | Gas distributor and slurry bed reactor and crude carbinol synthetic system both comprising same |
| CN102872769B (en) * | 2012-09-28 | 2015-04-22 | 神华集团有限责任公司 | Gas distributor and slurry bed reactor and crude carbinol synthetic system both comprising same |
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| CN101036865A (en) | 2007-09-19 |
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