CN101209403A - Method and equipment for liquid-solid continuously separation for slurry state bed reactor - Google Patents
Method and equipment for liquid-solid continuously separation for slurry state bed reactor Download PDFInfo
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- CN101209403A CN101209403A CNA2006101696735A CN200610169673A CN101209403A CN 101209403 A CN101209403 A CN 101209403A CN A2006101696735 A CNA2006101696735 A CN A2006101696735A CN 200610169673 A CN200610169673 A CN 200610169673A CN 101209403 A CN101209403 A CN 101209403A
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Abstract
The invention discloses a method and a piece of equipment which are used for continuously separating liquid and solid of a serum-bed reactor. The contact reaction between materials and catalyst particles takes place in a serum-bed reactor, and suspension serum after the reaction is guided into a separation unit which comprises an inclined-plate settlement vessel and quickly separated into supernatant and concentrated serum in the inclined-plate settlement vessel, wherein, the concentrated serum returns to the reactor for continuing to participate in the reaction, and the supernatant flows upward into an upper part of the inclined-plate settlement vessel along gaps between the plates and is exhausted. The method provided by the invention implements the continuous separation and circular utilization of solid catalyst particles and liquid products in a smaller operation space and improves settlement efficiency. The equipment provided by the invention is applicable for separating suspension serum with smaller catalyst particles and larger liquid viscosity, occupies small space and has high separation efficiency.
Description
Technical field
The present invention relates to method and apparatus that solia particle is separated from liquid, more particularly, relate to a kind of method and apparatus that paste state bed reactor liquid and solid particle separate continuously that is used for.
Background technology
Paste state bed reactor is a kind of gas-liquid commonly used (slurry) haptoreaction equipment, has high liquid storage amount.For the very big catalytic reaction process of reaction heat, use paste state bed reactor can remove reaction heat effectively, the isothermal operation of realization response device guarantees the normal operation of reactor, has therefore obtained extensive use in current chemical process.
In paste state bed reactor,, generally adopt tens microns even more fine grain catalyst, how effectively to realize liquid-solid separation after the reaction, become the key technology in using slurry attitude bed course of reaction in order to eliminate diffusion influence.Paste state bed reactor generally adopts the method for sedimentation, filtration to realize liquid-solid separation at present, for the catalyst with magnetic, explores the technology of utilizing magnetic to separate and separates.
US6068760, WO02/097007A2 all disclose and have adopted sedimentation techniques to realize the method for liquid-solid separation in paste state bed reactor, reacted slurries are drawn reactor, behind a sedimentation pipe, slurries enter settling tank and carry out sedimentation, supernatant liquor is discharged as product, and the thick slurry Returning reactor circulation of a large amount of catalyst granules is contained in lower floor.
The disclosed separation method of EP 1405664A1 is that reacted slurries are directly introduced settling tank, sedimentation is provided with baffle plate in irritating, and height of baffle plate is higher than liquid level in the settling tank, therefore after slurry stream is crossed the slit of baffle plate and tank base, clear liquid slowly rises and flows out above settling tank, and contains the outlet Returning reactor main body of the underflow of particle in the settling tank bottom.
Advantage such as that though sedimentation device has is simple in structure, operating flexibility is big, operating cost is low; but when being applied to starch attitude bed reaction system; because catalyst granules is less and fluid viscosity is bigger; infall process is very slow; in order to improve separative efficiency; just need the very big sedimentation device of volume, and guarantee enough sedimentation times.Sedimentation techniques are that the separating effect of the littler catalyst granules of several microns or particle diameter is not good for particle diameter in addition.Particularly require to realize the paste state bed reactor that solid-liquid separates continuously, because the device area is limited, and need measure such as insulation, the use of common subsider is restricted.
CN1433838A discloses the method that the sedimentation separation unit is set in reactor body, and applies high-intensity magnetic field to quicken liquid-solid separating rate in the bottom of sedimentation unit.Caused the most of area and the space of equipment to be taken by sedimentation device, production efficiency is lower; Because Fischer-Tropsch synthesis device diameter is quite big, thereby magnetic field device is difficult in and produces uniform magnetic field in the reactor, and the equipment heaviness involves great expense, and can't carry out demagnetization to stop the reunion of magnetization catalyst to producing magnetized catalyst, influence the normal running of reactor.
WO 94/16807 discloses in reactor the method for using filter assemblies to realize liquid-solid separation, in case but catalyst granules stops up filter assemblies, the regeneration difficulty of filter assemblies then, thereby be unsuitable for large-scale continuous production.
CN1589957A discloses at inside reactor the one-level separative element has been set, the secondary separative element is set outside reactor realizes the method for liquid-solid separation, and the continued operation of back flush unit to realize filtering is set outside reactor, so not only taken the reaction compartment in the reactor, also cause the device structure complexity, operate complicated.
Inclined plate settler has utilized the shallow layer settling theory, one group of inclination thin plate parallel to each other is installed in that common subsider is inner, and when suspension slurry flow through gap between the thin plate, particle carried out sedimentation separation, under the situation of identical device volume, has increased settling area.Because each gap all is an independently sedimentation unit, particle as long as touch on the swash plate below it, will rely on gravity to glide along swash plate in the process of sedimentation, has shortened settling height.
Summary of the invention
The method and apparatus that provides a kind of liquid that is used for paste state bed reactor and solid particle to separate continuously is provided on the basis of existing technology.
A kind of liquid-solid continuous separation method that is used for paste state bed reactor, raw material and catalyst granules haptoreaction in paste state bed reactor, the suspension slurry that contains catalyst granules after the reaction is introduced separative element, described separative element comprises inclined plate settler, suspension slurry is introduced inclined plate settler, in inclined plate settler, be separated into supernatant liquor and concentrated slurry fast, the concentrated slurry Returning reactor continues to participate in reaction, and supernatant liquor travels up to the top of inclined plate settler and discharges along the space between plate.
In the method provided by the invention, described separative element preferably is provided with preprocessor before inclined plate settler, the suspension slurry that will contain catalyst granules is introduced preprocessor, the gas of carrying secretly in the suspension slurry separates with suspension slurry herein, isolated gas Returning reactor top, isolated suspension slurry flow into inclined plate settler by the preprocessor bottom and further separate.
In the method provided by the invention, described separative element can be placed on the outside of reactor, also can be placed on the inside of reactor.When being placed on reactor outside, the preprocessor top of separative element and the gas compartment on reactor top are connected through pipeline, are convenient to discharge the gas on preprocessor top.
Introduce the feeding manner that suspension slurry can adopt top charging, underfeed and cross-feed by preprocessor to inclined plate settler, the mode of wherein preferred cross-feed, be that suspended nitride flows into inclined plate settler from the preprocessor bottom transverse earlier, flow up into capable sedimentation separation then.
The quantity of separative element is according to the output of fluid product in the paste state bed reactor, the volume of separative element, and solid content and the decision of fluid product target solid content in the suspension slurry.When reactor needs long-term operation, a plurality of separative elements can be set, by switching the continuous quiet run of implement device.
When the solid content of the suspension slurry of handling is higher (the volume percentage is greater than 5%), can increase the volume of preprocessor, at first isolate large-size particles by free settling, and suitably improve the upright position of preprocessor leakage fluid dram 13, reduce the slurry solid content that flows into inclined plate settler, thereby give full play to the effect of inclined plate settler, improve separative efficiency.
In order to prevent through after the long period running, being deposited on inclined plate settler edge, the gusset and in other local solid particle back mixing worsens infall process, flusher can be set in settler, when the solid holdup that flows out clear liquid does not reach when requiring, utilize flusher to extract slurries and wash cleaning, guarantee effective operation of separative element.
When needs obtain the lower fluid product of solid content, can further adopt means such as filtration, High-gradient Magnetic separation, supercritical fluid extraction that isolated fluid product is further handled.
A kind of solid-liquid separating equipment that is used for paste state bed reactor, comprise preprocessor and inclined plate settler, one group of parallel inclination thin plate of the inner placement of inclined plate settler is characterized in that these thin plates equidistantly connect by gusset, and the angle of thin plate and level is 30～80 °, preferred 45～70 °; Vertical interval h is 0.01～0.3 meter between plate, preferred 0.02～0.10 meter.
In the equipment provided by the invention, the thin plate of inclined plate settler can be dull and stereotyped, can be bent plate also, as be placed on the curved ellipse in the cylinder, conical plate etc.
When described thin plate when being dull and stereotyped, the long l/h of plate is 10～50 relatively, and is preferred 15～25, and the relative wide b/h of plate is 10～40, preferred 10～25, and wherein 1 display plate is long, and the h display plate is wide.
When adopting bent plate in cylindrical device, the radius of cylindrical device is 0.2～4 meter, preferred 0.5～2.5 meter.
The advantage of separation method provided by the invention is:
Method provided by the invention is applied to starch attitude bed reaction system with inclined plate settler, in less operating space, realized solid catalyst particle separate continuously with liquid form product, recycling, improved settling efficiency, from embodiment as seen, the solid volume percentage composition is less than 0.1% in the fluid product, the cutting particle diameter is 5 μ m, and separative efficiency is 98%.Preprocessor is set before inclined plate settler can realizes gas and react separating of back suspension slurry, and slurries are carried out initial gross separation, further improved separative efficiency.
The advantage that is used to starch the inclined plate settler of attitude bed reaction system provided by the invention is:
Be applicable to the separation of the suspension slurry that catalyst granules is less and fluid viscosity is bigger, it is little to take up room, the separative efficiency height.
Description of drawings
Fig. 1 is placed on the separation method schematic diagram of reactor outside for separative element;
Fig. 2 is placed on the separation method schematic diagram of inside reactor for separative element.
The specific embodiment
Specify a kind of liquid-solid continuous separation method that is used for paste state bed reactor provided by the invention below in conjunction with accompanying drawing, but therefore the present invention is not restricted.
Fig. 1 is placed on the separation method schematic diagram of reactor outside for separative element, as seen from Figure 1, reaction raw materials (gaseous state or liquid state) is introduced in the reactor 1 through pipeline 7, in the process that rises with reactor 1 in catalyst solid particle haptoreaction, generate product, unreacted gas is discharged reactor by pipeline 8.Reacted slurries are introduced separative element 2 through pipeline 9, separative element 2 is divided into preprocessor 3 and inclined plate settler 4 by baffle plate 6, slurries flow velocity in preprocessor 3 slows down, and the gas of carrying secretly is assembled on top, the gas compartment through pipeline 10 Returning reactors 1 top; And the slurries that removed gas flow into inclined plate settler 4 by bottom opening 13, solid particle in the slurries drops on the surface of swash plate 5 by settlement action herein, gravitate is along the bottom that slides to inclined plate settler 4 under the wooden partition, the concentrated slurry that forms continues to participate in reaction through pipeline 12 Returning reactors 1, clear liquid then travels up to the top of inclined plate settler 4 along the space between plate, discharge through pipeline 11.
Fig. 2 is placed on the separation method schematic diagram of inside reactor for separative element, and the preprocessor top is connected with the reactor head gas compartment as seen from the figure.In the case, the slurries in the reactor 1 enter preprocessor 3 through the pan feeding aperture 14 of separative element 2 sidewalls, the gas compartment that the gas of preprocessor 3 top enrichments directly enters reactor 1 top.The slurries that removed gas laterally flow into inclined plate settler 4 by preprocessor 3 bottom leakage fluid drams 13, realize Separation of Solid and Liquid at inclined plate settler 4, isolated clear liquid is discharged reactor 1 through pipeline 11, and the concentrated slurry of inclined plate settler 4 bottoms continues to participate in reaction through pipeline 12 Returning reactors 1.
The following examples will give further instruction to method provided by the invention, but not thereby limiting the invention.
Embodiment
The flow process that the paste state bed reactor solid-liquid separates continuously as shown in Figure 1, wherein to adopt the plate inclination angle be one group of parallel flat of 50 ° to inclined plate settler, vertical interval is 0.05m between plate.The suspension slurry of discharging in the reactor is introduced the preseparator of separative element, the bigger catalyst sedimentation of grain diameter is in the preprocessor bottom, isolated than underflow liquid Returning reactor continuation participation reaction, isolated gas Returning reactor top, all the other suspension slurries flow into inclined plate settler and further separate in the preprocessor bottom; Isolated clear liquid is a liquid form product in the inclined plate settler.Through the weight method analysis: the solid masses percentage composition is less than 0.1% in the clear liquid, and the cutting particle diameter is 5 μ m, and it is 98% that swash plate is distinguished from efficient.
Claims (10)
1. liquid-solid continuous separation method that is used for paste state bed reactor, raw material and catalyst granules haptoreaction in paste state bed reactor, the suspension slurry that contains catalyst granules after the reaction is introduced separative element, in separative element, be divided into supernatant liquor and concentrated slurry, the concentrated slurry Returning reactor continues to participate in reaction, it is characterized in that described separative element comprises inclined plate settler, suspension slurry is separated into supernatant liquor and concentrated slurry fast in inclined plate settler, the concentrated slurry Returning reactor continues to participate in reaction, and clear liquid travels up to the top of inclined plate settler and discharges along the space between plate.
2. according to the method for claim 1, it is characterized in that described separative element comprises preprocessor and inclined plate settler, suspension slurry is introduced the preprocessor of separative element, the gas of carrying secretly in the suspension slurry separates with suspension slurry herein, isolated gas Returning reactor top, isolated suspension slurry flow into inclined plate settler by the pretreating zone bottom and further separate.
3. according to the method for claim 2, it is characterized in that described separative element is placed on the outside of paste state bed reactor, preprocessor top and paste state bed reactor top are communicated with through pipeline.
4. according to the method for claim 2, it is characterized in that described separative element is placed on the inside of paste state bed reactor.
5. according to claim 2,3 or 4 method, it is characterized in that described suspension slurry flows into inclined plate settler from the preprocessor bottom transverse.
6. liquid-solid separation equipment that is used for paste state bed reactor, it is characterized in that this equipment comprises preprocessor and inclined plate settler, one group of parallel inclination thin plate of the inner placement of inclined plate settler, thin plate equidistantly connects by gusset, and the angle of thin plate and level is 30～80 °, and vertical interval h is 0.01～0.3 meter between plate.
7. according to the equipment of claim 6, it is characterized in that the angle of described thin plate and level is 45～70 °, vertical interval h is 0.02～0.1 meter between plate.
8. according to the equipment of claim 6, it is characterized in that described thin plate is flat board or bent plate.
9. according to the equipment of claim 8, it is characterized in that the long l/h of the relative plate of described flat board is 15～25, the wide b/h of plate is 10～25 relatively.
10. according to the equipment of claim 9, it is characterized in that the long l/h of relative plate of described flat board is 10～50, the wide b/h of plate is 10～40 relatively.
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| CN101747228A (en) * | 2008-11-28 | 2010-06-23 | 中国石油化工股份有限公司 | The Ammoximation reaction of a kind of ketone or aldehyde |
| CN101327036B (en) * | 2008-07-19 | 2010-10-13 | 石河子大学 | Detaching mechanism for excess material after catsup processing |
| CN101733045B (en) * | 2008-11-14 | 2012-04-18 | 中国石油化工股份有限公司 | Solid-liquid separation device and solid-liquid separation method for slurry bed reactor |
| CN102553343A (en) * | 2011-12-20 | 2012-07-11 | 赛鼎工程有限公司 | Method and device for continuously separating catalyst of synthetic fluid fuel in slurry bed from product |
| CN102985150A (en) * | 2010-06-30 | 2013-03-20 | 戴维加工技术有限公司 | Process and system for the separation of solid carboxylic acid fines |
| CN102049222B (en) * | 2009-10-29 | 2013-06-05 | 中国石油化工股份有限公司 | Application method of loop slurry reactor adopting novel filtration module |
| CN103747861A (en) * | 2011-06-24 | 2014-04-23 | 安格斯化学公司 | Process and apparatus for production and filtration of aminoalcohols using a continuous stirred tank slurry reactor |
| CN103769014A (en) * | 2014-01-24 | 2014-05-07 | 神华集团有限责任公司 | Fluidized bed reactor |
| CN103962070A (en) * | 2013-01-31 | 2014-08-06 | 中国科学院上海高等研究院 | Slurry bed reaction method |
| CN110478951A (en) * | 2019-09-17 | 2019-11-22 | 四川北方红光特种化工有限公司 | A kind of technique and catalyst settler increasing catalyst sedimentation |
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| CN101327036B (en) * | 2008-07-19 | 2010-10-13 | 石河子大学 | Detaching mechanism for excess material after catsup processing |
| CN101733045B (en) * | 2008-11-14 | 2012-04-18 | 中国石油化工股份有限公司 | Solid-liquid separation device and solid-liquid separation method for slurry bed reactor |
| CN101747228B (en) * | 2008-11-28 | 2013-06-26 | 中国石油化工股份有限公司 | Ammoximation reaction of ketone or aldehyde |
| CN101747228A (en) * | 2008-11-28 | 2010-06-23 | 中国石油化工股份有限公司 | The Ammoximation reaction of a kind of ketone or aldehyde |
| CN102049222B (en) * | 2009-10-29 | 2013-06-05 | 中国石油化工股份有限公司 | Application method of loop slurry reactor adopting novel filtration module |
| CN102985150A (en) * | 2010-06-30 | 2013-03-20 | 戴维加工技术有限公司 | Process and system for the separation of solid carboxylic acid fines |
| US9211518B2 (en) | 2011-06-24 | 2015-12-15 | Angus Chemical Company | Process and apparatus for production and filtration of aminoalcohols using a continuous stirred tank slurry reactor |
| CN103747861B (en) * | 2011-06-24 | 2016-08-31 | 安格斯化学公司 | Use the method and apparatus being used for producing and filter amino alcohol of continuous stirred tank slurry reactor |
| CN103747861A (en) * | 2011-06-24 | 2014-04-23 | 安格斯化学公司 | Process and apparatus for production and filtration of aminoalcohols using a continuous stirred tank slurry reactor |
| CN102553343A (en) * | 2011-12-20 | 2012-07-11 | 赛鼎工程有限公司 | Method and device for continuously separating catalyst of synthetic fluid fuel in slurry bed from product |
| CN102553343B (en) * | 2011-12-20 | 2014-05-28 | 赛鼎工程有限公司 | Method and device for continuously separating catalyst of synthetic fluid fuel in slurry bed from product |
| CN103962070A (en) * | 2013-01-31 | 2014-08-06 | 中国科学院上海高等研究院 | Slurry bed reaction method |
| CN103962070B (en) * | 2013-01-31 | 2017-11-28 | 中国科学院上海高等研究院 | A kind of method for carrying out slurry reactor |
| CN103769014B (en) * | 2014-01-24 | 2016-07-20 | 神华集团有限责任公司 | A kind of fluidized bed reactor |
| CN103769014A (en) * | 2014-01-24 | 2014-05-07 | 神华集团有限责任公司 | Fluidized bed reactor |
| CN110478951A (en) * | 2019-09-17 | 2019-11-22 | 四川北方红光特种化工有限公司 | A kind of technique and catalyst settler increasing catalyst sedimentation |
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| CN111991905A (en) * | 2020-07-30 | 2020-11-27 | 国家能源集团宁夏煤业有限责任公司 | Method and device for solid-liquid separation of slurry discharged from slurry bed |
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| CN112604327B (en) * | 2020-11-30 | 2021-06-29 | 新疆农业大学 | Desilting basin |
| CN113019268A (en) * | 2021-03-04 | 2021-06-25 | 中国石油大学(北京) | Inertia settler and gas-liquid-solid three-phase reaction system comprising same |
| CN113082977A (en) * | 2021-04-06 | 2021-07-09 | 江苏舒源空调制造有限公司 | Efficient waste gas treatment system and process |
| CN113082977B (en) * | 2021-04-06 | 2021-11-30 | 江苏舒源空调制造有限公司 | Efficient waste gas treatment system and process |
| CN115364530A (en) * | 2022-09-13 | 2022-11-22 | 新特能源股份有限公司 | Polysilicon slag slurry settling device and recovery system |
| CN115364530B (en) * | 2022-09-13 | 2024-04-30 | 新特能源股份有限公司 | Polycrystalline silicon slurry sedimentation device and recovery system |
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