CN1233451C - Contiuous industrial reactor of slurry state bed in gas, liquid and solid three phases - Google Patents
Contiuous industrial reactor of slurry state bed in gas, liquid and solid three phases Download PDFInfo
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- CN1233451C CN1233451C CN 03151109 CN03151109A CN1233451C CN 1233451 C CN1233451 C CN 1233451C CN 03151109 CN03151109 CN 03151109 CN 03151109 A CN03151109 A CN 03151109A CN 1233451 C CN1233451 C CN 1233451C
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- 239000007787 solid Substances 0.000 title claims abstract description 48
- 239000007788 liquid Substances 0.000 title claims abstract description 27
- 239000002002 slurry Substances 0.000 title claims abstract description 25
- 239000007789 gas Substances 0.000 title claims description 38
- 238000000926 separation method Methods 0.000 claims abstract description 16
- 238000009826 distribution Methods 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 6
- 238000004804 winding Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000002826 coolant Substances 0.000 claims description 2
- 239000000498 cooling water Substances 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 239000008258 liquid foam Substances 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 239000000428 dust Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 description 10
- 238000003786 synthesis reaction Methods 0.000 description 10
- 239000012071 phase Substances 0.000 description 8
- 238000001914 filtration Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 239000000725 suspension Substances 0.000 description 3
- 241000628997 Flos Species 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000007792 gaseous phase Substances 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007701 flash-distillation Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000008570 general process Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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Abstract
The present invention relates to a gas to liquid to solid three-phase slurry state bed industrial reactor continuously operated. The reactor comprises an inlet gas distribution component which is composed of an inlet gas distribution pipe and unevenly distributes gas, one layer or a plurality of layers of heat exchange pipe components for heating/cooling a bed layer, one layer or a plurality of layers of liquid-solid separation device components which can be automatically cleaned, and an outlet dust removing demister component for removing liquid foam and solid entrainment. Compared with the prior art, the present invention has low energy consumption and solves the problem of clogging or counterflow. Temperature and liquid level are controlled very well to stably and continuously operate the reactor.
Description
Technical field
The present invention relates to chemical industry equipment device field, be specifically related to a kind of three phase slurry bed industrial reactor that can continued operation.
Background technology
Three-phase (gas-liquid-solid) paste state bed reactor has obtained extensive use in chemical process.In existing literature and patent, report is arranged more.Provide a kind of gas-liquid-solid three-phase loop reactor as Chinese patent 99127184.X; Chinese patent 99813677.8 and 97227653.X provide a kind of phase reactor of jetting type; What Chinese patent 02117348.6 was narrated is the spouted bed bioreactor that does not relate to catalytic process, and Chinese patent 93236114.5 and 94241250.8 is the decanter type reactor; Chinese patent 94222395.0 and 97227653.X are the mechanical agitation tank reactor.
The phase reactor that in Chinese patent 98124535.8, provides a kind of air-flow bubbling to suspend, this reactor consists of the following components: the bottom tower head of a tape entry nozzle, one or more heat exchanging segments that are immersed in the synthesis stage; The several rows of outlet nozzle that goes out suspension, the barrier film of an outlet nozzle of discharging unreacting gas and one group of lateral inclination is with the dedusting foam removal.
Reactor described in the above patent has following problem if be used for the industrial reaction process: circulating, jetting type or spouted hearth reactor energy consumption are bigger, and are easy to cause the wearing and tearing (spouted bed is unsuitable for catalytic reaction process) of catalyst; The decanter type reactor is suitable for batch process, and the general processes that are used for wastewater treatment should not be done continuous production more; The mechanical agitation tank reactor is because energy consumption greatly to the catalyst abrasion height, is commonly used for the laboratory reaction device.
And for Chinese patent 98124535.8 described air-flow bubbling suspension reactors, the deficiency of existence is: the gas access nozzle is arranged on reactor bottom, and gas passes through gas distributor from bottom to top, results in blockage easily or adverse current when dying breaking down; Solid suspension is discharged and is handled, and if desired catalyst is returned, and needs bigger energy consumption and causes mechanical wear.These will be unfavorable for continuous industrial production.
Summary of the invention
Purpose of the present invention is exactly the gas-liquid-solid three-phase slurry attitude bed industrial reactor that a kind of continued operation is provided for the defective that overcomes above-mentioned prior art existence, and this reactor can be realized the industrial operation of steady and continuous by effective structure setting.
Purpose of the present invention can be achieved through the following technical solutions: a kind of gas-liquid-solid three-phase slurry attitude bed industrial reactor of continued operation, it is characterized in that this reactor comprises following four part parts at least: inlet gas distributed elements, heat exchanger tube parts, liquid-solid separator parts, outlet dedusting demister parts;
Described inlet gas distributed elements is the one group of gas distribution tube (1) that is arranged on reactor bottom, this gas distribution tube (1) is gone up perforate and is disposed nozzle (2), this nozzle (2) evenly distributes on reactor cross section, and be downwards or lateral openings, the size of nozzle (2) internal diameter should guarantee that gas passes through pressure drop that each nozzle of distributor pipe produced between 0.01MPa～0.1MPa;
Described heat exchanger tube parts are one or more layers heat exchanger tube, and heat exchanger tube is taked two kinds of patterns: a kind of is the heat exchanger tube (4) of helical disk tubular type, is the multi-turn coil pipe concentric with reactor, and heat transferring medium is spiral from top to bottom flowing in coil pipe; Another kind is a winding type multipass heat exchanger tube (4 '), and many vertical heat exchanger tubes are combined by connecting bend up and down, every group of circuitous up and down flowing of heat exchange liquid in pipe, and the heat exchanger tube of this pattern is provided with many group heat exchanger tubes on same cross section;
Described liquid-solid separator parts are one or more layers liquid-solid separation device (7) that places in the reactor, and the liquid that this device maybe needs fluid product to replace separates with solid particle; Every layer of liquid-solid separation device comprises one or more groups liquid-solid resolution element, every group of liquid-solid resolution element is made up of one or more liquid-solid resolution element arranged side by side again, liquid-solid resolution element arranged side by side is combined by two connecting pipes up and down, is connected on the outer house steward of reactor; In order to prevent the obstruction of liquid-solid separation device, be provided with the recoil cleaning that special recoil control program regularly carries out liquid-solid resolution element, simultaneously, in order to control liquid level, the liquid-solid resolution element quantity that comes into operation by the recoil control program is adjustable, and the recoil medium is liquid or gas;
Partly for being arranged at the dedusting demister (11) of the baffle plate type in top, it links to each other with outlet described outlet dedusting demister, and the built-in online flusher of this dedusting demister (11) washes with nitrogen or reacting gas.
The inlet house steward of described inlet gas distributed elements is provided with check (non-return) valve (14) near the reactor place; A high pressure N is set behind check (non-return) valve
2Accident blow line (15) also is provided with check (non-return) valve (16) on this pipeline (15).
Described reactor bottom also is provided with outer coil pipe, feeds cooling water when carrying out exothermic reaction keeping certain temperature, if when carrying out the endothermic reaction, then this coil pipe feeds steam to keep the operating temperature of reactor.
Institute's flow media is a cooling medium in the described heat exchanger tube parts, or heat medium; For winding type multipass heat exchanger tube, heat medium uses the high-temp liquid heat-conducting medium.
Described reactor middle part is provided with an online interpolation mouth of pipe (10), adds the fresh catalyst slurries inward, or as the liquid of inert media; Reactor bottom is provided with an online discharging mouth of pipe (3), is used for the exhaust catalyst slurries, cooperates with the operation of online interpolation pipe, to keep certain liquid level and to keep the stable of concentration of slurry.
Compared with prior art, energy consumption of the present invention is low, has solved obstruction or reflux problem, and temperature and liquid level control are good, has realized the stable and continuous operation of reactor.
Description of drawings
Fig. 1 is the structural representation of the commerical test scale reaction device of a synthesis gas producing fluid fluid fuel;
Fig. 2 is the flow chart of whole reactor system;
Fig. 3 is another type structure schematic diagram of reactor heat exchanger tube parts.
The specific embodiment
The following examples are synthesis gas producing fluid fluid fuel process, and promptly the Fischer-Tropsch building-up process commerical test scale reaction device example now is illustrated in conjunction with Fig. 1～Fig. 3.
The Fischer-Tropsch synthesis device is the synthesis gas that utilizes based on hydrogen and carbon monoxide, under the effect of catalyst and carry out Fischer-Tropsch under 200～250 ℃, the operating condition of 2.0～5.0MPa in slurry attitude bed and synthesize, generates a series of hydrocarbon compound.Hydrocarbon compound obtains condensate and paraffin after Quench, flash distillation, separation, filtration.Wherein paraffin is as the liquid medium in the reactor, is again the important products of synthesizing, and therefore need be reclaimed, but catalyst need be stayed in the reactor.
The Fischer-Tropsch building-up process is strong exothermic process, so temperature of reactor need be controlled well.Need enough effective heat exchange measures on the one hand, need the distribution of gas of circulation in the reactor even on the other hand.
As Fig. 1, this synthesis reactor is divided into six sections, comprises two-layer heat exchanger tube 4 and two-layer liquid-solid separation device 7, is connected with flange between each section.
Wherein, 1 is the inlet gas distributor pipe, and 2 is the nozzle on the gas distribution tube, 3 is the online floss holes of slurries, 4 is heat exchanger tube, and 5 is the heat transferring medium import, and 6 are the heat transferring medium outlet, 7 is liquid-solid separation device, 8 are the recoil inlet, and 9 is filtering outlet, and 10 are the online inlet that adds of slurries, 11 are the dedusting demister, and 12 is gaseous phase outlet.
Synthesis gas enters from gas access distributor pipe 1, on distributor pipe 1, distribute, nozzle 2 is under shed, and the size of designed nozzle inside diameter has guaranteed that gas is not less than 0.05MPa by distributor pipe 1 injection differential pressure, thereby gas can be entered in the slurry attitude bed uniformly.
From the gas access distributed elements up is ground floor heat exchanger tube 4, and this heat exchanger tube pattern is a spiral coil, for the Fischer-Tropsch synthesis of heat release, walks boiler feedwater in the coil pipe, by boiler feedwater bed is cooled off.But, when device is driven, also can feed steam in the coil pipe and come slurries are carried out preheating.
Ground floor heat exchanger tube 4 is a ground floor liquid-solid separation device 7 up, is made up of 6 groups of filter elements, and every group of filter element is a tube filtering element.Each tube filtering element upper orifice is a backflush liquid inlet 8, lower nozzle is for filtering back liquid outlet 9, filtering outlet 9/ recoil inlet 8 is equipped with valve outside reactor, controlled by other special filtration/recoil program, guarantees that the liquid level of reactor maintains certain level.
Ground floor liquid-solid separation device 7 up is second layer heat exchange coil 4 and second layer liquid-solid separation device 7 successively, and its structure configuration effect is identical with ground floor.
In reactor second layer heat exchanger tube 4 lower ends an online inlet 10 that adds of catalyst slurry is set, as required, the fresh catalyst slurries is added.The slurries of the online floss hole 3 of catalyst slurry bottom this process need cooperate discharge and carry out, to keep certain liquid level and to guarantee the stable of catalyst concn.Because catalyst is to reduce in other reduction reactor, can be in good time carry out online updating, guaranteed the stable of average activity.
Liquid level is in second layer liquid-solid separation device 7 position more up during normal running, up be one section gas-liquid separation space again, the gas of carrying liquid and small amount of solid secretly enters the baffle plate type dedusting demister 11 at top by this section space, carry the gas and the deflection plate bump of liquid foam secretly, most drops and solid are caught, and gas is discharged by gaseous phase outlet 12.The built-in online flusher of dedusting demister is by washing the mouth of pipe 13 usefulness high pressure nitrogens to dedusting demister periodic flushing.This dedusting demister 11 can will be removed greater than the drop more than 8 microns 100% and not occur stopping up, and pressure drop is less than 0.005MPa.
Catalyst particle mean size in this reactor is 50 μ m, and slurry weight concentration is 45%.This covering device operation tempus semestre, distribution of gas in order, temperature control steadily, stopping up does not appear in liquid-solid separation device, average activity is stable, at 240 ℃, 3.0MPa, the inlet linear speed is under the synthesis condition of 0.45m/s, H
2All the time maintain 80～90% level with the total conversion of CO.
Fig. 2 is the reactor assembly figure of present embodiment, and wherein 14,16 is check (non-return) valve, has prevented back flow of gas; 15 is the high pressure nitrogen emergency pipe line, the situation of distributor pipe spray nozzle clogging when being used to handle synthesis gas interruption or pressure instability.
Fig. 3 is the example of another pattern of heat exchanger tube, for the multipass heat exchanger tube 4 of winding type '.This heat exchanger components is combined by connecting bend 17 up and down by four vertical heat exchanger tubes, and liquid is circuitous up and down flowing in every group of heat exchanger tube.The mouth of pipe 5 ' be the medium import wherein, the mouth of pipe 6 ' be media outlet.This pattern heat exchanger tube uses in an other cover commerical test device, realizes better temperature control effect though increased processing cost.
Claims (5)
1. the gas-liquid-solid three-phase of continued operation slurry attitude bed industrial reactor is characterized in that this reactor comprises following four part parts at least: inlet gas distributed elements, heat exchanger tube parts, liquid-solid separator parts, outlet dedusting demister parts;
Described inlet gas distributed elements is the one group of gas distribution tube (1) that is arranged on reactor bottom, this gas distribution tube (1) is gone up perforate and is disposed nozzle (2), this nozzle (2) evenly distributes on reactor cross section, and be downwards or lateral openings, the size of nozzle (2) internal diameter should guarantee that gas passes through pressure drop that each nozzle of distributor pipe produced between 0.01MPa～0.1MPa;
Described heat exchanger tube parts are one or more layers heat exchanger tube, and heat exchanger tube is taked two kinds of patterns: a kind of is the heat exchanger tube (4) of helical disk tubular type, is the multi-turn coil pipe concentric with reactor, and heat transferring medium is spiral from top to bottom flowing in coil pipe; Another kind is a winding type multipass heat exchanger tube (4 '), and many vertical heat exchanger tubes are combined by connecting bend up and down, every group of circuitous up and down flowing of heat exchange liquid in pipe, and the heat exchanger tube of this pattern is provided with many group heat exchanger tubes on same cross section;
Described liquid-solid separator parts are one or more layers liquid-solid separation device (7) that places in the reactor, and the liquid that this device maybe needs fluid product to replace separates with solid particle; Every layer of liquid-solid separation device comprises one or more groups liquid-solid resolution element, every group of liquid-solid resolution element is made up of one or more liquid-solid resolution element arranged side by side again, liquid-solid resolution element arranged side by side is combined by two connecting pipes up and down, is connected on the outer house steward of reactor; In order to prevent the obstruction of liquid-solid separation device, be provided with the recoil cleaning that special recoil control program regularly carries out liquid-solid resolution element, simultaneously, in order to control liquid level, the liquid-solid resolution element quantity that comes into operation by the recoil control program is adjustable, and the recoil medium is liquid or gas;
Partly for being arranged at the dedusting demister (11) of the baffle plate type in top, it links to each other with outlet described outlet dedusting demister, and the built-in online flusher of this dedusting demister (11) washes with nitrogen or reacting gas.
2. the gas-liquid-solid three-phase of a kind of continued operation according to claim 1 slurry attitude bed industrial reactor is characterized in that the inlet house steward of described inlet gas distributed elements is provided with check (non-return) valve (14) near the reactor place; A high pressure N is set behind check (non-return) valve
2Accident blow line (15) also is provided with check (non-return) valve (16) on this pipeline (15).
3. the gas-liquid-solid three-phase of a kind of continued operation according to claim 1 is starched attitude bed industrial reactor, it is characterized in that, described reactor bottom also is provided with outer coil pipe, feed cooling water when carrying out exothermic reaction to keep certain temperature, if when carrying out the endothermic reaction, then this coil pipe feeds steam to keep the operating temperature of reactor.
4. the gas-liquid-solid three-phase of a kind of continued operation according to claim 1 slurry attitude bed industrial reactor is characterized in that institute's flow media is a cooling medium in the described heat exchanger tube parts, or heat medium; For winding type multipass heat exchanger tube, heat medium uses the high-temp liquid heat-conducting medium.
5. the gas-liquid-solid three-phase of a kind of continued operation according to claim 1 is starched attitude bed industrial reactor, it is characterized in that, described reactor middle part is provided with an online interpolation mouth of pipe (10), adds the fresh catalyst slurries inward, perhaps as the liquid of inert media; Reactor bottom is provided with an online discharging mouth of pipe (3), is used for the exhaust catalyst slurries, cooperates with the operation of online interpolation pipe, to keep certain liquid level and to keep the stable of concentration of slurry.
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| CN 03151109 CN1233451C (en) | 2003-09-22 | 2003-09-22 | Contiuous industrial reactor of slurry state bed in gas, liquid and solid three phases |
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| CN 03151109 CN1233451C (en) | 2003-09-22 | 2003-09-22 | Contiuous industrial reactor of slurry state bed in gas, liquid and solid three phases |
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| CN1233451C true CN1233451C (en) | 2005-12-28 |
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Cited By (1)
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| WO2022078427A1 (en) | 2020-10-14 | 2022-04-21 | 中国石油化工股份有限公司 | Method and system for preparing hydrogen peroxide |
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| CN102441351B (en) * | 2010-10-12 | 2015-09-02 | 中国石油化工股份有限公司 | A kind of slurry bed ft synthetic reactor |
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| CN105833801A (en) * | 2016-05-27 | 2016-08-10 | 北京神雾环境能源科技集团股份有限公司 | Gas foam remover for acetylene hydrogenation type ethylene preparation trickle bed |
| CN105833806A (en) * | 2016-05-27 | 2016-08-10 | 北京神雾环境能源科技集团股份有限公司 | Gas foam remover for acetylene hydrogenation type ethylene preparation three-phase fluidized bed |
| CN105833803A (en) * | 2016-05-27 | 2016-08-10 | 北京神雾环境能源科技集团股份有限公司 | Gas foam remover for acetylene hydrogenation type ethylene preparation packing bubbling bed |
| CA3021930A1 (en) * | 2016-06-02 | 2017-12-07 | The Petroleum Oil And Gas Corporation Of South Africa (Soc) Ltd | Slurry bubble column reactor for a fischer-tropsch process |
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| CN107254327B (en) * | 2017-06-05 | 2021-12-17 | 中石化宁波工程有限公司 | Fischer-Tropsch synthetic oil process |
| CN111790319B (en) * | 2019-04-08 | 2022-08-30 | 国家能源投资集团有限责任公司 | Slurry bed reactor, system and application thereof and Fischer-Tropsch synthesis method |
| CN112546968B (en) * | 2020-12-02 | 2022-04-19 | 中国科学院广州能源研究所 | Three-phase reactor and method applied to hydrodeoxygenation refining of biological aviation oil |
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2003
- 2003-09-22 CN CN 03151109 patent/CN1233451C/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022078427A1 (en) | 2020-10-14 | 2022-04-21 | 中国石油化工股份有限公司 | Method and system for preparing hydrogen peroxide |
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Application publication date: 20050330 Assignee: SHAANXI FUTURE ENERGY CHEMICAL CO.,LTD. Assignor: Shanghai Yankuang Energy Sources Technology Research & Development Co.,Ltd. Contract record no.: 2012310000147 Denomination of invention: Contiuous industrial reactor of slurry state bed in gas, liquid and solid three phases Granted publication date: 20051228 License type: Common License Record date: 20120813 |
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Application publication date: 20050330 Assignee: Sichuan Yilong masukuni Energy Co.,Ltd. Assignor: Shanghai Yankuang Energy Sources Technology Research & Development Co.,Ltd. Contract record no.: 2014310000012 Denomination of invention: Contiuous industrial reactor of slurry state bed in gas, liquid and solid three phases Granted publication date: 20051228 License type: Common License Record date: 20140121 |
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Inventor after: Sun Qiwen Inventor after: Zhu Jicheng Inventor after: Geng Jiahuai Inventor after: Wang Xin Inventor after: Han Hui Inventor before: Zhu Jicheng Inventor before: Geng Jiahuai Inventor before: Wang Xin Inventor before: Han Hui |
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Free format text: CORRECT: INVENTOR; FROM: ZHU JICHENG GENG JIAHUAI WANG XIN HAN HUI TO: SUN QIWEN ZHU JICHENG GENG JIAHUAI WANG XIN HAN HUI |
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| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20051228 |