CN101352620A - Method and apparatus for micro hydrocyclone separation of MTO quench water and water of water-washing factory, and for concentration of fine catalyst in the same - Google Patents
Method and apparatus for micro hydrocyclone separation of MTO quench water and water of water-washing factory, and for concentration of fine catalyst in the same Download PDFInfo
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- CN101352620A CN101352620A CNA200810042662XA CN200810042662A CN101352620A CN 101352620 A CN101352620 A CN 101352620A CN A200810042662X A CNA200810042662X A CN A200810042662XA CN 200810042662 A CN200810042662 A CN 200810042662A CN 101352620 A CN101352620 A CN 101352620A
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Abstract
The invention provides a micro-vortex flow concentration method used for fine catalyst in MTO quenching water and washing water, comprising the steps as follows: micro-vortex flow separation of MTO quenching water is carried out so as to carry out the concentration processing on the contained catalyst and micro-vortex flow separation of MTO washing water is carried out so as to carry out the concentration processing of the contained catalyst. The invention also provides a micro-vortex flow concentration device used for the fine catalyst in the MTO quenching water and washing water.
Description
Technical field
The invention belongs to coal transformation technology field, relate to the method and apparatus that adopts little eddy flow method that contained solid catalyst in methanol-to-olefins (MTO) technology chilled water (chw) and the washing water is concentrated.Because valuable catalyst granules enters water body in chilling and water-washing process,, must carry out liquid-solid concentrating to chilled water (chw) and washing water in order to reclaim catalyst.The present invention is suitable for handling the concentrated fine particle process that comprises MTO technology chilled water (chw), washing water, also is fit to the concentration process of other micro-subparticle or drop.
Background technology
Catalyst is very general in the application of each industrial circles such as chemical industry, petrochemical industry, biochemical industry, its active component is precious metal often, therefore the cost of making catalyst is very high, how to recycle the most important thing that catalyst is engineering design to greatest extent.MTO is the abbreviation of methanol-to-olefins, and cardinal principle is to produce methyl alcohol from coal through synthesis gas, is low-carbon alkene (main component is ethene and propylene) by methanol conversion again, is applied to other chemical article and industrial goods then.The MTO technological process comprises that mainly reactive moieties, product purify part and product separating part.Reactive moieties comprises reactor and regenerator, and product purification portion branch comprises quench tower, water scrubber, caustic wash tower and drying tower, and all the other are the product separating part.The reactor that MTO is commonly used is a fluidized-bed reactor, all exists with gas phase at reactor internal reaction thing methyl alcohol and olefin product.
US 6166282 discloses a kind of MTO fluidized-bed reactor, in reactor head one group of cyclone separator is installed, and with separating catalyst solid particle from the product discharge currents, prevents that catalyst granules is entrained with reactor.Though reaction gas flow is by several cyclone separators, but still have catalyst granules and leave reactor with the product discharge currents, these catalyst particles separate with the reacting gas product with washing water with chilled water (chw) respectively in quench tower and water scrubber, enter water circulation system with chilled water (chw) and washing water, thereby cause the wearing and tearing of upstream device to stop up, shortened the service cycle of device.
In MTO technology, after leaving reactor, the product discharge currents that carries catalyst enters the quench tower chilling.In quench tower, water and methanol condensed are liquid, and olefin product remains gas, and most of catalyst granules enters in the water and discharges quench tower with chilled water (chw), so is rich in catalyst granules in the chilled water (chw).In order further to remove the catalyst dust of carrying secretly in the product gas flow, the olefin product air-flow will enter the water scrubber washing, and catalyst is wherein thoroughly removed, and catalyst dust enters in the washing water.In order to reclaim catalyst, decontamination cycle water is necessary chilled water (chw) is carried out liquid-solid the separation, the catalyst concentration slurry with washing water simultaneously.
US 5744680A discloses and has a kind ofly produced the method for lighter hydrocarbons by oxide, wherein contains catalyst stream and discharges from the wet scrubbing step.US 6870072 also discloses and has utilized the wet scrubbing district to remove catalyst in the product discharge currents.
US 0234281 and CN 1942558A disclose a kind of one or more solid-liquid cyclone separators or cyclone hydraulic separators that adopts a cover serial or parallel connection combined running at the MTO chilled water (chw), and catalyst reclaims use after separating.The product stream of discharging from reactor has passed through several vapor-solid cyclonic separation in reactor, so the particle diameter of catalyst granules very little (1-20 micron, 80% below 10 microns) in the MTO chilled water (chw), and the particle in the washing water can littler (below 5 microns).But, conventional solid-liquid whirlwind or effective seizure particle diameter of cyclone hydraulic separators are about the 5-10 micron, can only remove because of running the catalyst that decreases under the non-normal working conditions such as inefficacy of solid-liquid cyclone separator or operation failure, normal operating conditions for cyclone separator then can not or be difficult to the solid particle of removal below 2 microns, so conventional solid-liquid whirlwind or cyclone hydraulic separators can only be used as when running the catalyst accident and use, and can not play Expected Results under the normal operation.
Therefore, this area presses for the method that a kind of catalyst granules to carrying secretly in MTO chilled water (chw), the washing water that can remove the solid particle below 2 microns in normal operation concentrates of developing.
Summary of the invention
The invention provides a kind of method and device new, that concentrate trickle catalyst in MTO chilled water (chw), the washing water, overcome the defective that prior art exists.
On the one hand, the invention provides the little eddy flow method for concentration of trickle catalyst in a kind of MTO chilled water (chw), the washing water, this method comprises:
The MTO chilled water (chw) is carried out little rotational flow separation, so that the catalyst that wherein contains is carried out concentration; And
MTO washing water is carried out little rotational flow separation, so that the catalyst that wherein contains is carried out concentration.
One preferred embodiment in, the operating temperature of described MTO chilled water (chw) is 95-115 ℃, catalyst content is 100-1000mg/L, catalyst particle size is the 1-20 micron, the water-filling density of catalyst is 1300-1500kg/m
3
Another preferred embodiment in, the density of described MTO chilled water (chw) is 900-930kg/m
3, viscosity is the 0.15-0.35 centipoise.
Another preferred embodiment in, the operating temperature of described MTO washing water is 30-50 ℃, catalyst content is 70-800mg/L, catalyst particle size is the 1-10 micron.
Another preferred embodiment in, the density of described MTO washing water is 923-953kg/m
3, viscosity is the 0.551-0.751 centipoise.
On the other hand, the invention provides the little eddy flow enrichment facility of trickle catalyst in a kind of MTO chilled water (chw), the washing water, this device comprises:
Be connected with quench tower, be used for the MTO chilled water (chw) is carried out little rotational flow separation, the catalyst that wherein contains is carried out little cyclone separator group of concentration; Be connected with described quench tower, be used for the olefin product after separating through quench tower is washed, further to remove the water scrubber of remaining catalyst granules in the product discharge currents; Be connected with described water scrubber, be used for MTO washing water is carried out little rotational flow separation, the catalyst that wherein contains is carried out little cyclone separator group of concentration.
One preferred embodiment in, described little cyclone separator group is made up of single-stage, two-stage or more multistage little cyclone separator.
Another preferred embodiment in, described little cyclone separator is composed in parallel by single, two or more eddy flow core pipes.
Another preferred embodiment in, the pressure loss of the little cyclone separator group of described chilled water (chw) is 0.1-0.25MPa.
Another preferred embodiment in, the pressure loss of the little cyclone separator group of described washing water is 0.15-0.25MPa.
Description of drawings
Fig. 1 is the schematic diagram according to the MTO process catalyst concentration flow path of one embodiment of the present invention.
The specific embodiment
The present inventor is through finding after the extensive and deep research, and is big for MTO chilled water (chw), this operation flux of washing water, the solid-liquid system that solids content is low, and the most effective, the most inexpensive method is to adopt cyclone separator; But because conventional eddy flow, the cut diameter of cyclone hydraulic separators is greater than 5 microns, can not or be difficult to remove the solid particle below 2 microns in normal operation, therefore, invented and adopted little cyclone separation process that the catalyst granules in chilled water (chw) and the washing water is concentrated, because the diameter of little eddy flow core pipe is littler several times even tens times than the diameter of common cyclone separator, therefore the solid particle centrifugal force suffered in the Disengagement zone compare with common cyclone separator much bigger, so the separative efficiency of little eddy flow core pipe also just is much higher than common eddy flow, cyclone hydraulic separators.Based on above-mentioned discovery, the present invention is accomplished.
Generate based on the low-carbon alkene of ethene, propylene and a large amount of water in the MTO course of reaction.Product and unreacted methanol are carried little amount of catalyst with the form of gas together and are left reactor.After the product discharge currents entered quench tower cooling, catalyst granules entered in the water, and a part is discharged from the quench tower bottom, was called water at the bottom of the chilled water (chw), and another part is discharged from the top of quench tower.Olefin product is washed further to remove remaining catalyst to water scrubber behind the quench tower chilling, and catalyst is discharged at the bottom of water scrubber with water, enters in the washing water.Under normal operation, the catalyst content in the product discharge currents seldom, particle grain size is also very little, so catalyst concentration is very low in chilled water (chw) and the washing water.But because there are density contrast in catalyst and water, at quench tower inner catalyst solid particle skewness in the axial direction, at the bottom of tower, catalyst concn is high more, and particle diameter is big more.Catalyst concn from the chilled water (chw) that extract out on quench tower top is very low, does not need Separation of Solid and Liquid directly to loop back quench tower after the cooler cooling.All discharge technology at the bottom of the tower with chilled water (chw) and compare, this technology has several advantages: 1. reduce the treating capacity of solid-liquid separating equipment, reduced equipment and operating cost; 2. can increase the solid content of water at the bottom of the quench tower, help the raising of solid-liquid separation efficiency.Water is through after little cyclone separator group at the bottom of the chilled water (chw), the part stripping tower stripping separation of methanol of purifying waste water, a part as chilling agent return quench tower, purify waste water through the washing water after separating and also return water scrubber and recycle, two bursts of rich catalyst stream concentrate does further processing.
In a first aspect of the present invention, a kind of method that adopts little eddy flow method that contained solid catalyst in MTO technology chilled water (chw) and the washing water is concentrated is provided, this method comprises:
The little amount of catalyst that water contains at the bottom of adopting little cyclone separator to quench tower is carried out concentration, and chilled water (chw) after a purification part is carried out stripping to stripper, another part after cooler is lowered the temperature as chilling agent return quench tower; And
The little amount of catalyst that water contains at the bottom of adopting little cyclone separator to water scrubber is carried out concentration, and the washing water after the purification returns water scrubber after the cooler cooling.
Preferably, the operating temperature of described chilled water (chw) is about 95-115 ℃, and catalyst content is about 100-1000mg/L, and catalyst particle size is about the 1-20 micron.
Preferably, the operating temperature of described washing water is about 30-50 ℃, and catalyst content is about 70-800mg/L, and catalyst particle size is about the 1-10 micron.
Preferably, the density of described chilled water (chw) is about 900-930kg/m
3, viscosity is about the 0.15-0.35 centipoise.
Preferably, the density of described washing water is about 923-953kg/m
3, viscosity is about the 0.551-0.751 centipoise.
Preferably, the water-filling density of the catalyst in the described chilled water (chw) is about 1300-1500kg/m
3
In a second aspect of the present invention, a kind of device that adopts little eddy flow method that contained solid catalyst in MTO technology chilled water (chw) and the washing water is concentrated is provided, this device comprises:
Be connected with MTO reactor 1, be used for the resulting product discharge currents that carries catalyst granules of MTO reaction is carried out the quench tower 2 of chilling, so that olefin removal moisture content, methyl alcohol and catalyst in the product, methyl alcohol and most of catalyst granules enter in the chilled water (chw); Be connected with described quench tower 2, be used for water scrubber 3 that the olefin product after separating through quench tower 2 is washed, in order to further to remove remaining catalyst granules in the product discharge currents; Be connected with described quench tower 2, be used for water at the bottom of the chilled water (chw) is carried out Separation of Solid and Liquid, with the little cyclone separator group of the chilled water (chw) of thickened solid catalyst 4-1; Be connected with the little cyclone separator group of described chilled water (chw) 4-1, be used for chilled water (chw) cooler 5-1 that the chilling that obtains through Separation of Solid and Liquid is purified waste water and cooled, in order to realize the recycling of water; Be connected with described chilled water (chw) cooler 5-1, be used for the chilling water pump 6-1 that purifies waste water and be transported to quench tower 2 through the chilling of chilled water (chw) cooler 5-1 cooling; Be used for carrying out Separation of Solid and Liquid, with the little cyclone separator group of the washing water 4-2 of solid catalyst in the condensed water wash water, in order to remove the catalyst fines in the washing water to washing water-bed water; Be connected with the little cyclone separator group of described washing water 4-2, be used for the washing water cooler 5-2 that the water washing cleaning water that obtains is cooled after separating; And be connected with described washing water cooler 5-2, be used for the water washing cleaning water through washing water cooler 5-2 cooling is transported to the washing water pump 6-2 of water scrubber 3.
Preferably, described chilled water (chw), the little cyclone separator group of washing water are made up of one or more little cyclone separators.
Preferably, described little cyclone separator is made up of some cover eddy flow core pipes.
Preferably, the entrance velocity of the little cyclone separator group of described chilled water (chw) is about the 5-10 meter per second, and the pressure loss is about 0.1-0.25MPa, and the water inlet gauge pressure is about 0.9-1.3MPa.
Preferably, the entrance velocity of the little cyclone separator group of described washing water is about the 8-15 meter per second, and the pressure loss is about 0.15-0.25MPa, and the water inlet gauge pressure is about 1.2-1.6MPa.
Preferably, the content of catalyst is about 100-1000mg/L the water at the bottom of the quench tower that quench tower comes out, and water-filling density is about 1300-1500kg/m
3, particle grain size is about 1-20 μ m.(operating pressure is about 0.9-1.3MPa to contain the chilled water (chw) of minor amount of catalyst particles, operating temperature is about 20-80 ℃) enter little cyclone separator group with the speed of about 8-10 meter per second, under action of centrifugal force, realize Separation of Solid and Liquid, separate through one or more little cyclone separators, the content of rich catalyst pulp inner catalyst can reach more than the 40g/L.
Preferably, at the bottom of the water scrubber in the water content of catalyst be lower than chilled water (chw), be about 70-800mg/L; Particle grain size also is less than the particle diameter of catalyst in the chilled water (chw), is about 1-10 μ m.Entrance velocity is a key factor that influences separative efficiency, and entrance velocity is big more, and the suffered centrifugal force of particle is also big more, the easy more separation of two-phase; But entrance velocity is big more, and the required pressure reduction of rotational flow separation equipment is also big more, and energy consumption is also just big more.In order to make the catalyst in the washing water effectively to separate, the entrance velocity (about 8-15 meter per second) of the little cyclone separator group of washing water is greater than the entrance velocity of the little cyclone separator group of chilled water (chw).(operating pressure is about 1.2-1.6MPa to contain the washing water of trace catalyst particle, operating temperature is about 30-50 ℃) enter little cyclone separator group with the speed of about 8-15 meter per second, under action of centrifugal force, realize Separation of Solid and Liquid, separate through one or several little cyclone separator, the content of rich catalyst pulp inner catalyst can reach more than the 36g/L.
Preferably, method and apparatus of the present invention also can be applied to concentrating of trickle catalyst granules the chilled water (chw) of MTP (methyl alcohol system third is rare) and OTO (producing lighter hydrocarbons from oxygenatedchemicals) technology and the washing water.
Below referring to accompanying drawing.
Fig. 1 is the schematic diagram according to the MTO process catalyst concentration flow path of one embodiment of the present invention.As shown in Figure 1, methyl alcohol added in the MTO reactor 1 react, generate based on the low-carbon alkene of ethene, propylene and a large amount of water; Product and unreacted methanol are carried little amount of catalyst with the form of gas together and are left MTO reactor 1; After the product discharge currents entered quench tower 2 cooling, catalyst granules entered in the water, and a part is discharged from the bottom of quench tower 2, was called water at the bottom of the chilled water (chw), and another part is discharged from the top of quench tower 2; Olefin product is washed further to remove remaining catalyst to water scrubber 3 behind quench tower 2 chillings, and catalyst is discharged from the bottom of water scrubber 3 with water, enters in the washing water; Water is through little cyclone separator group 4-1 at the bottom of the chilled water (chw), after 4-1 ' separates, and the part stripping tower stripping separation of methanol of purifying waste water, a part cools through chilled water (chw) cooler 5-1 as the chilling agent, and returns quench tower 2 after the chilling water pump 6-1 supercharging; Washing water is through little cyclone separator group 4-2, and behind the 4-2 ', a part cools through washing water cooler 5-2, and returns water scrubber 3 after the washing water pump 6-2 supercharging.
The little eddy flow of single-stage concentrates 20-30 doubly, the second level concentrates 20-30 doubly, (illustrate: the two poles of the earth, cyclone front can reach 20-30 thickening efficiency doubly to the underflow maximum concentration less than 50%, but don't work what grade cyclones, catalyst concentration is necessarily less than 50% in the final concentrate, and this is by cyclone decision itself).
The major advantage of method and apparatus of the present invention is:
The present invention adopts little cyclone separator to carry out dense to contained catalyst in MTO technology chilled water (chw) and the washing water Contracting has the outstanding advantages such as equipment cost is cheap, separative efficiency is high, the operation cycle is long.
All quote in this application as a reference at all documents that the present invention mentions, just as each piece document Quoted separately as a reference such. Should be understood that in addition after having read above-mentioned instruction content of the present invention, Those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within this Shen equally Please the appended claims limited range.
Claims (10)
1. the little eddy flow method for concentration of trickle catalyst in a MTO chilled water (chw), the washing water, this method comprises:
The MTO chilled water (chw) is carried out little rotational flow separation, so that the catalyst that wherein contains is carried out concentration; And
MTO washing water is carried out little rotational flow separation, so that the catalyst that wherein contains is carried out concentration.
2. the method for claim 1 is characterized in that, the operating temperature of described MTO chilled water (chw) is 95-115 ℃, and catalyst content is 100-1000mg/L, and catalyst particle size is the 1-20 micron, and the water-filling density of catalyst is 1300-1500kg/m
3
3. method as claimed in claim 1 or 2 is characterized in that, the density of described MTO chilled water (chw) is 900-930kg/m
3, viscosity is the 0.15-0.35 centipoise.
4. the method for claim 1 is characterized in that, the operating temperature of described MTO washing water is 30-50 ℃, and catalyst content is 70-800mg/L, and catalyst particle size is the 1-10 micron.
5. as claim 1 or 4 described methods, it is characterized in that the density of described MTO washing water is 923-953kg/m
3, viscosity is the 0.551-0.751 centipoise.
6. the little eddy flow enrichment facility of trickle catalyst in a MTO chilled water (chw), the washing water, this device comprises:
Be connected with quench tower (2), be used for the MTO chilled water (chw) is carried out little rotational flow separation, the catalyst that wherein contains is carried out little cyclone separator group (4-1) of concentration; Be connected with described quench tower (2), be used for the olefin product after separating through quench tower (2) is washed, with the water scrubber (3) of further removing remaining catalyst granules in the product discharge currents; Be connected with described water scrubber (3), be used for MTO washing water is carried out little rotational flow separation, the catalyst that wherein contains is carried out little cyclone separator group (4-2) of concentration.
7. device as claimed in claim 6 is characterized in that, described little cyclone separator group is made up of single-stage, two-stage or more multistage little cyclone separator.
8. device as claimed in claim 6 is characterized in that, described little cyclone separator is composed in parallel by single, two or more eddy flow core pipes.
9. as each described device among the claim 6-8, it is characterized in that the pressure loss of described little cyclone separator group (4-1) is 0.1-0.25MPa.
10. as each described device among the claim 6-8, it is characterized in that the pressure loss of described little cyclone separator group (4-2) is 0.15-0.25MPa.
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| CN102093153A (en) * | 2010-11-05 | 2011-06-15 | 华东理工大学 | Optimal combination method and device for purifying and separating MTO (Methanol To Olefins) reaction gas containing catalyst micropowder |
| CN102190544A (en) * | 2010-03-03 | 2011-09-21 | 中国石油化工股份有限公司 | Method for rapidly cooling reaction product of oxygen-containing compound produced alkene |
| CN102603539A (en) * | 2012-02-07 | 2012-07-25 | 上海华畅环保设备发展有限公司 | Method and device for recycling catalyst particles in crude toluene diamine |
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| CN108328761B (en) * | 2017-08-29 | 2023-08-29 | 华东理工大学 | Method and device for prolonging continuous operation period of MTO water washing process |
| CN107382654A (en) * | 2017-09-01 | 2017-11-24 | 上海华畅环保设备发展有限公司 | Methanol-to-olefins chilled water (chw) ebullated bed separation method and device |
| CN107382654B (en) * | 2017-09-01 | 2023-08-25 | 上海华畅环保设备发展有限公司 | Separation method and device for quenching water boiling bed for preparing olefin from methanol |
| WO2022056776A1 (en) * | 2020-09-17 | 2022-03-24 | 华东理工大学 | Fluidized bed separation method and device for methanol-to-olefins quenched water |
| WO2022056777A1 (en) * | 2020-09-17 | 2022-03-24 | 华东理工大学 | Method and apparatus for prolonging continuous operation period of methanol-to-olefins water washing process |
| RU2814431C1 (en) * | 2020-09-17 | 2024-02-28 | Ист Чайна Юниверсити Оф Сайенс Энд Текнолоджи | Method and device for prolonging continuous mode of washing process with water when converting methanol to olefins |
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Application publication date: 20090128 |