CN104415716B - Slurry bed reactor as well as application method thereof - Google Patents
Slurry bed reactor as well as application method thereof Download PDFInfo
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- CN104415716B CN104415716B CN201310400051.9A CN201310400051A CN104415716B CN 104415716 B CN104415716 B CN 104415716B CN 201310400051 A CN201310400051 A CN 201310400051A CN 104415716 B CN104415716 B CN 104415716B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
- B01J8/22—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid
Abstract
The invention relates to a slurry bed reactor as well as an application method thereof. The slurry bed reactor comprises a cover (12), an expanding section (13) which is arranged on the lower part of the cover (12) with the pipe diameter which is greater than the cover and a draft tube (11) which is arranged inside the expanding section (13) with the pipe diameter which is less than the cover (12), wherein the bottom opening of the cover (12) runs into the expanding section (13), the outer wall of the cover (12) is connected with the top of the expanding section (13), the upper opening of the draft tube (11) runs into the cover (12) and the lower part of the draft tube (11) is opened. The slurry bed reactor provided by the invention is simple and practical in structure, convenient to operate, few in occupied area and easy to enlarge, can be continuously and stably operated, and can be suitable for a reaction system of a relatively large granular catalyst.
Description
Technical field
The present invention relates to a kind of slurry reactor device and its application process, consolidate or gas-liquid-solid response system for liquid.
Background technology
Paste state bed reactor is a kind of consersion unit of conventional gas-liquid-solid three-phase contact.Liquid be continuous phase, gas and
Solid is dispersion phase.Gas, as the power of mixing and lifting, catalyst is suspended and is reacted in the liquid phase.Due to there is no machine
Tool stirs, thus can No leakage run under high pressure.The feature of paste state bed reactor is by gas sparging strengthening fluid, promotees
Enter the transmission of the matter and energy between gas-liquid two-phase.Catalyst generally all adopts finely grained catalyst, can effectively eliminate internal diffusion
Impact to reaction, has very high catalytic efficiency, paste state bed reactor is easily realized isothermal operation, avoided the occurrence of bed simultaneously
Focus, beneficial to improve reaction selectivity the features such as.
Although paste state bed reactor has lot of advantages, the application in petrochemical process is not extensive, restricts it
The topmost reason of application is product and the separation problem of catalyst granules, serosity transportation problem and for solving these
Problem and a series of engineering problems of bringing.Propose many improvement projects for this Chinese scholars.
GB2403728A discloses the method separation product filtering outside a kind of employing device and catalyst, but this process route is relatively
Long.And, extract the conveying of suspension and the conveying returning paste state bed reactor out from paste state bed reactor, and be filtered
Catalyst slurry conveying power all to be provided by pump, not only energy consumption is higher, during easily cause catalyst granules
Breakage, increased the difficulty of solid-liquor separation, macrocyclic operation brings inconvenience to reactor.
CN102049222A proposes a kind of paste state bed reactor arranging filter assemblies inside tedge, but this filtration
The dismounting of device is difficult, also increases the complexity of inside reactor structure simultaneously, and the maintenance of filter is changed to slurry bed system
Operation impact is very greatly it is difficult to maximize.In addition, not considering that serosity deaerates, bubbles in serosity, increased serum recycle pipeline
Vapour lock, simultaneously gas occupy filter media surface, filter efficiency is low.
CN1233451C discloses one kind containing gas-distributing component, heat exchanger components, solid-liquor separation part and foam removal part
Paste state bed reactor, but structure of reactor is complicated, and operation is complicated, and the reaction that multiple inner members not only occupy in reactor is empty
Between so that height for reactor is higher, and have an effect on the control of liquid flow pattern in slurry bed system.
CN101314120A discloses a kind of slurry bed circulatory flow reactor including tedge and down-comer.Wherein, rise
Pipe is made up of the decanting zone that reaction zone and caliber expand.Have aperture between decanting zone and reaction zone to connect, this reactor is suitable for
In the situation that catalyst granules is larger.Although this reactor is provided with extension diameter section decanting zone, it is confined to the diameter of decanting zone, catalysis
The sedimentation of agent granule not exclusively, still needs to set up external filter, increased cost of investment.
Analyzed from above, the liquid phase conveying of paste state bed reactor, solid-liquor separation, gas-liquid separation are several must to solve
Key issue.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of slurry reactor device of integrated form and a kind of application slurry
Bed realizes gas-liquid-solid three-phase successive reaction, detached application process.
The paste state bed reactor that the present invention provides, including calotte 12, is located at calotte 12 bottom, caliber is more than the expanding of calotte
Section 13 and be located inside extension diameter section 13, caliber is less than the guide shell 11 of calotte 12, the bottom opening of described calotte 12 stretches into expansion
Inside footpath section 13, described calotte 12 outer wall is connected with extension diameter section 13 top, and the upper opening of described guide shell 11 stretches into cap
Inside cover 12, described guide shell 11 lower openings.
The application process of the above-mentioned paste state bed reactor that the present invention provides, liquid phase feed and/or phase feed are passed through respectively
Fluid inlet 1 and gas phase import 2 enter paste state bed reactor bottom, contact concurrently with solid catalyst particle in guide shell 11
Raw reaction, under gas push, product enters gas-liquid separation in calotte 12 by guide shell 11 open top, isolates
Gas is discharged by gaseous phase outlet 4, and the serosity containing solid catalyst particle flows downwardly into extension diameter section by the open top of guide shell 11
13, solid catalyst particle settles in extension diameter section, forms the serosity rich in solid catalyst particle and reaction clear liquid, serosity is by expanding
Footpath section 13 bottom enters guide shell 11 and again participates in reacting, and reaction clear liquid goes out device from liquid-phase outlet 3.
In the method that the present invention provides, gas is in guide shell（11）Interior superficial gas velocity is 0.01～1.0m/s.
In the method that the present invention provides, the mean diameter of described solid catalyst particle is 100～5000 microns, preferably
200～1000 microns.
The having the beneficial effect that of paste state bed reactor and methods for using them that the present invention provides：
The paste state bed reactor integrated level that the present invention provides is high, structure is simple, small investment, and floor space is few, easy to operate.
Reaction completes in guide shell, and guide shell top is connected with calotte, completes gas-liquid separation in calotte, and serosity removing gas can have
Effect avoids the vapour lock in feed-line；Calotte bottom opening is communicated with extension diameter section, and serosity, in the sedimentation of extension diameter section, is realized liquid and admittedly divided
From clear liquid goes out device, and the serosity rich in catalyst granules is in inside reactor circulation it is adaptable to the slurry of greater particle size catalyst
Bed reaction system, preferably 100～5000 microns of catalyst granules particle diameter.The maximization of achievable slurry reactor device and long week
Phase stable operation.In addition, the paste state bed reactor and methods for using them that the present invention provides need not additionally arrange catalyst slurry filtering
Device.
Brief description
Fig. 1 is the structural representation of the slurry reactor device of the present invention.
Wherein：1- fluid inlet, 2- gas phase import, 3- liquid-phase outlet, 4- gaseous phase outlet, 5- reacts clear liquid, 6- reaction slurry
Liquid, 11- guide shell, 12- calotte, 13- extension diameter section.
Specific embodiment
Slurry reactor device and its specific embodiment of application process that the detailed description below present invention provides：
A kind of paste state bed reactor, including calotte 12, is located at calotte 12 bottom, caliber is more than extension diameter section 13 and of calotte
Inside extension diameter section 13, caliber be less than the guide shell 11 of calotte 12, the bottom opening of described calotte 12 stretches into extension diameter section 13
Inside, described calotte 12 outer wall is connected with extension diameter section 13 top, and the upper opening of described guide shell 11 stretches in calotte 12
Portion, described guide shell lower openings are in reactor so that the inside of extension diameter section 13 communicates in bottom with inside guide shell 11.
In the paste state bed reactor that the present invention provides, the described bottom setting gas phase import 2 of extension diameter section 13 and liquid phase are entered
Mouth 1, described extension diameter section 13 side wall arranges liquid-phase outlet 3, and described calotte 12 top arranges gaseous phase outlet 4.Wherein, described
Fluid inlet 1 and gas phase import 2 are respectively one or more.
Preferably, the internal diameter of described guide shell 11 and calotte 12 is than for 1:1.1～10.
Preferably, the internal diameter of described extension diameter section 13 and calotte 12 is than for 1.1～10：1.
Preferably, the height that described guide shell 11 stretches in calotte 12 accounts for the 1/10～9/10 of calotte 12 total height.
Preferably, described liquid-phase outlet 3 be located at extension diameter section 13 height from down to up 50%～100% at.
Preferably, the bottom opening of described calotte 12 is located at the liquid-phase outlet 3 same level height of extension diameter section 13 or is less than
The level height of liquid-phase outlet 3.
Preferably, described fluid inlet setting liquid distribution trough, described gas phase import arranges gas distributor.
Preferably, described guide shell 11 is internal and/or extension diameter section 13 inside arranges heat exchanger.
The application process of the above-mentioned paste state bed reactor that the present invention provides, liquid phase feed and/or phase feed are passed through respectively
Fluid inlet 1 and gas phase import 2 enter paste state bed reactor bottom, contact concurrently with solid catalyst particle in guide shell 11
Raw reaction, under gas push, product enters gas-liquid separation in calotte 12, the gas isolated by guide shell 11 open top
Body is discharged by gaseous phase outlet 4, and the serosity containing solid catalyst particle flows downwardly into extension diameter section 13 by the open top of guide shell 11,
Solid catalyst particle settles in extension diameter section, forms the serosity rich in solid catalyst particle and reaction clear liquid, serosity is by expanding
Section 13 bottom enters guide shell 11 and again participates in reacting, and reaction clear liquid goes out device from liquid-phase outlet 3.
Preferably, superficial gas velocity in guide shell 11 for the gas is 0.01～1.0m/s.
Preferably, the mean diameter of described solid catalyst particle be 100～5000 microns, more preferably 200～1000
Micron.
The paste state bed reactor and methods for using them that the present invention provides, arranges heat exchanger, according to reaction preferably in reaction tube
The size of heat, can be used for taking out reaction heat, controlling reaction temperature, to ensure reaction efficiency.Gaseous phase outlet at cap top it
Before, gas scrubbing section is set inside or outside calotte, can effectively prevent solid catalyst particle from being taken out of by gas.
" top " of the container mentioned in description refers to the position of the 0-50% of container height from top to bottom, container " under
Portion " refers to the position of the 50%-1000% of container from top to bottom, and " bottom " of the container mentioned refers to the 90%- of container from top to bottom
100% position.
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.It should be appreciated that this place is retouched
The specific embodiment stated is merely to illustrate and explains the present invention, is not limited to the present invention.
Accompanying drawing 1 is the structural representation of the slurry reactor device of the present invention, and as shown in Figure 1, liquid charging stock passes through liquid
Phase import 1, gas raw material passes through gas phase import 2 and gas distributor enters in paste state bed reactor.Gas-liquid in guide shell 11
Contact with catalyst granules three and concurrently give birth to reaction, product enters in calotte 12 through guide shell 11 open top, in cap
In cover 12, gas-liquid is sufficiently separated, and gas is discharged from paste state bed reactor top through gaseous phase outlet 4.Slurry containing catalyst granules
Liquid is flowed downward by through the annular space space between guide shell 11 and calotte, enters in extension diameter section 13, catalyst granules is in extension diameter section
Settle in 13, form the serosity rich in catalyst granules and reaction clear liquid, serosity reenters guide shell from extension diameter section 13 bottom
Reaction is participated in 11；Reaction clear liquid is from liquid-phase outlet 3 ejector.Extension diameter section 13 can be provided with heat exchanger, by cold for recirculated water etc. Jie
Matter is passed through heat exchanger, takes reaction heat away.On extension diameter section 13 bottom or liquid phase feeding pipeline, catalyst charging hole, reactor can be set
Bottom can arrange catalyst emission mouth, and fresh catalyst can add reactor by catalyst charging hole, and dead catalyst passes through slurry
The catalyst emission mouth of state bed reactor bottom discharges reactor, catalyst add or take out can intermittently operated it is also possible to online
It is carried out continuously.
Further illustrate the present invention by the following examples, but the present invention is not therefore subject to any restriction.
Embodiment 1
Embodiment 1 illustrates paste state bed reactor and the application effect of present invention offer.
Paste state bed reactor using the present invention carries out hydrogen peroxide synthesis.Experimental provision is as shown in drawings.Wherein, water conservancy diversion
Cylinder Φ 150 × 12000, calotte Φ 300 × 1600, extension diameter section Φ 500 × 12500.Hydrogen and working solution are respectively from gas phase import 2
Enter reactor with fluid inlet 1, reaction temperature is adjusted by the heat exchanger in extension diameter section.In the presence of 60 DEG C, catalyst, work
Make the EAQ in liquid, tetrahydrochysene EAQ is hydrogenated the hydride generating anthrahydroquinone containing ethyl and tetrahydrochysene ethyl anthrahydroquinone.
In guide shell, superficial gas velocity is 0.15m/s.Product enters calotte area under the castering action of gas and carries out gas-liquid separation,
Gas discharges reactor through gaseous phase outlet, and the hydride containing catalyst granules enters extension diameter section by interior circulation and sinks
Fall, forms the serosity rich in catalyst granules and reaction clear liquid, and serosity enters guide shell from extension diameter section bottom and again participates in reacting,
Reaction clear liquid then goes out device from liquid-phase outlet, enters follow-up oxidation-extraction system.Reaction bar after stable operation 1500 hours
Part and result are summarized in table 1.
Wherein：Working solution contains EAQ, tetrahydrochysene EAQ, trioctyl phosphate, heavy aromatics.The concentration of general anthraquinone is
The volume ratio of 130～140g/l, heavy aromatics and trioctyl phosphate is 75:25.Wherein, general anthraquinone refers to EAQ and tetrahydrochysene ethyl
The summation of anthraquinone.
The preparation method of catalyst used is：
Serosity drying and moulding is mixed to get by boehmite, Ludox, boric acid powder and deionized water, at 600 DEG C
Catalyst carrier is obtained after roasting 8h and is distributed to and obtain oxidation state containing dipping, drying, roasting in Palladous chloride., the solution of Lanthanum (III) nitrate
Catalyst, is prepared with pure hydrogen reduction 4h under the conditions of 150 DEG C.220 microns of catalyst mean diameter, particle size range is 140-310
Micron.Catalyst consists of：Pd content 1.2 weight %, sial mass ratio is SiO2:Al2O3=1:4.
Hydrogen imitates assay method：Take 5mL hydride in separatory funnel, add the heavy aromatics of 10mL and the H of 20mL2SO4Molten
Liquid（H2SO4Volume ratio with water is 1:4）；O is led to in above-mentioned mixed solution2, till bubbling is oxidizing to glassy yellow or crocus
（About 10～15min）；With pure water extractive reaction liquid 4～5 times, about 20mL water every time；Use concentration 0.1mol/ in extract
The KMnO of L4Standard solution is titrated to blush, 30s colour-fast for terminal.Then hydrogen effect（gH2O2/L）=concentration of standard solution
(0.1mol/L) × standard solution volume (mL) × 17.01/5.
Table 1 synthesis hydroperoxidation condition and result
| Reaction temperature, DEG C | 60 |
| Reaction pressure, MPa | 0.3 |
| Working solution inlet amount, m3/h | 1.2 |
| H2Inlet amount, Nm3/h | 9.5 |
| Hydrogen is imitated, gH2O2/l | 12 |
Claims (10)
1. a kind of paste state bed reactor is it is characterised in that including calotte (12), being located at calotte (12) bottom, caliber more than calotte
Extension diameter section (13), and be located at the guide shell (11) that extension diameter section (13) is internal, caliber is less than calotte (12), described calotte (12)
Bottom opening stretch into that extension diameter section (13) is internal, described calotte (12) outer wall is connected with extension diameter section (13) top, and described leads
The upper opening of flow cartridge (11) stretches into that calotte (12) is internal, described guide shell (11) lower openings, described extension diameter section (13) with
The internal diameter of calotte (12) is than for 1.1～10：1；Bottom setting gas phase import (2) of described extension diameter section (13) and/or liquid phase are entered
Mouth (1), described extension diameter section (13) side wall arranges liquid-phase outlet (3), and described calotte (12) top arranges gaseous phase outlet (4)；
The bottom opening of described calotte (12) is located at extension diameter section (13) liquid-phase outlet (3) same level height or is less than liquid-phase outlet (3)
Level height.
2. paste state bed reactor according to claim 1 is it is characterised in that the internal diameter ratio of described guide shell (11) and calotte (12)
For 1：1.1～10.
3. the paste state bed reactor according to claim 1 or 2 is it is characterised in that described guide shell (11) stretches into calotte (12)
In height be calotte (12) total height 1/10～9/10.
4. the paste state bed reactor according to claim 1 or 2 is it is characterised in that described liquid-phase outlet (3) is located at extension diameter section
(13) height from down to up 50%～100% at.
5. the paste state bed reactor according to claim 1 or 2 is it is characterised in that described fluid inlet setting liquid distribution trough,
Described gas phase import setting gas distributor.
6. the paste state bed reactor according to claim 1 or 2 arranges heat exchange it is characterised in that described extension diameter section (13) is internal
Device.
7. the application process of any one paste state bed reactor of claim 1～6 is it is characterised in that liquid phase feed and/or gas phase are former
Material passes through fluid inlet (1) and gas phase import (2) entrance paste state bed reactor bottom respectively, in guide shell (11) and catalyst
Granule contacts and reacts, and under gas push, product enters gas in calotte (12) by guide shell (11) open top
Liquid separates, and the gas isolated is discharged by gaseous phase outlet (4), and the serosity containing catalyst granules is by the open top of guide shell (11)
Flow downwardly into extension diameter section (13), catalyst granules settles in extension diameter section, form the serosity rich in catalyst granules and reaction clear liquid,
Serosity enters guide shell (11) by extension diameter section (13) bottom and again participates in reacting, and reaction clear liquid goes out device from liquid-phase outlet (3).
8. method according to claim 7 it is characterised in that superficial gas velocity in guide shell (11) for the gas be 0.01～
1.0m/s.
9. the method according to claim 7 or 8 is it is characterised in that a diameter of 100～5000 microns of catalyst granules.
10. method according to claim 9 is it is characterised in that a diameter of 200～1000 microns of catalyst granules.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310400051.9A CN104415716B (en) | 2013-09-05 | 2013-09-05 | Slurry bed reactor as well as application method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310400051.9A CN104415716B (en) | 2013-09-05 | 2013-09-05 | Slurry bed reactor as well as application method thereof |
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| CN104415716A CN104415716A (en) | 2015-03-18 |
| CN104415716B true CN104415716B (en) | 2017-02-08 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106552577B (en) * | 2015-09-30 | 2018-07-31 | 中国石油化工股份有限公司 | A kind of multilayer guide shell bubbling reactor and its application method |
| CN115945155B (en) * | 2023-03-09 | 2023-05-12 | 北京赛科康仑环保科技有限公司 | Device and method for producing sodium bicarbonate |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2538416Y (en) * | 2001-08-20 | 2003-03-05 | 石油大学(华东) | Circulation reactor for hydrocracking process of heavy oil suspension bed |
| CN200977457Y (en) * | 2006-12-01 | 2007-11-21 | 平顶山工学院 | Novel diameter-variable type three-phase fluidized bed |
| CN201971790U (en) * | 2011-01-24 | 2011-09-14 | 中国石油化工股份有限公司 | Inward flow slurry bed reactor |
| CN201969548U (en) * | 2011-01-24 | 2011-09-14 | 中国石油化工股份有限公司 | Internal circulating-flow slurry bed reactor |
| CN203853075U (en) * | 2013-09-05 | 2014-10-01 | 中国石油化工股份有限公司 | Slurry bed reactor |
-
2013
- 2013-09-05 CN CN201310400051.9A patent/CN104415716B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2538416Y (en) * | 2001-08-20 | 2003-03-05 | 石油大学(华东) | Circulation reactor for hydrocracking process of heavy oil suspension bed |
| CN200977457Y (en) * | 2006-12-01 | 2007-11-21 | 平顶山工学院 | Novel diameter-variable type three-phase fluidized bed |
| CN201971790U (en) * | 2011-01-24 | 2011-09-14 | 中国石油化工股份有限公司 | Inward flow slurry bed reactor |
| CN201969548U (en) * | 2011-01-24 | 2011-09-14 | 中国石油化工股份有限公司 | Internal circulating-flow slurry bed reactor |
| CN203853075U (en) * | 2013-09-05 | 2014-10-01 | 中国石油化工股份有限公司 | Slurry bed reactor |
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