CN102441527B - Separation method for catalysts of different inactivation degrees - Google Patents
Separation method for catalysts of different inactivation degrees Download PDFInfo
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- CN102441527B CN102441527B CN201010509289.1A CN201010509289A CN102441527B CN 102441527 B CN102441527 B CN 102441527B CN 201010509289 A CN201010509289 A CN 201010509289A CN 102441527 B CN102441527 B CN 102441527B
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Abstract
The invention discloses a separation method for catalysts of different inactivation degrees. The method comprises the following steps of: firstly removing oil on unload catalysts to keep the catalysts in a free flow state; separating the catalysts of different inactivation degrees; arranging a vertical constant-speed separation passage; introducing the catalysts to be separated from the middle upper part of the vertical constant-speed separation passage by using a branch pipe in a slant downward direction; introducing air from the lower part of the vertical constant-speed separation passage by using a branch pipe in the slant upward direction; and communicating a top outlet of the vertical constant-speed separation passage with a cyclone separator, wherein a material recovered by the cyclone separator is a catalyst of light inactivation degree, and the material recovered at the bottom of the vertical constant-speed separation passage is a catalyst of heavy inactivation degree. By using the method, the high-activity and low-pollution catalyst can be recovered and reutilized; and the method can be continuously performed, is flexible in operation and is most suitable for separating discharge catalysts in a hydro-treatment process of a residual oil boiling bed.
Description
Technical field
The present invention relates to a kind of separation method of different level of deactivation catalyst, relate in particular to a kind of separation method of boiling bed residual oil hydrogenation catalyst of different level of deactivation.
Background technology
The heavy oil deep processing is to alleviate one of approach of petroleum resources deficiency, and the heavy-oil hydrogenation technology is to solve the effective method of heavy oil deep processing.Existing heavy-oil hydrogenation technology is divided into fixed bed hydrogenation processing, boiling bed hydrogenation cracking, floating bed hydrocracking and moving bed hydrotreatment technology Four types.Wherein the fixed bed hydrogenation treatment technology is the most ripe relatively, is most widely used.But its adaptability to raw material is poor and limitation is outstanding day by day.The boiling bed residual oil hydrocracking technology have to substantially good without pressure drop, uniformity of temperature profile, mass transfer and heat transfer in feedstock oil strong adaptability, reactor, catalyst can add online and discharge, catalyst utilization is high, service cycle is long, install the advantages such as flexible operation, constantly developed in recent years.
In the boiling bed hydrogenation processing procedure, feedstock oil and hydrogen enter reactor from reactor bottom with certain speed, make the interior catalyst of reactor in swelling state.In order to maintain certain reactivity, need constantly or termly to draw off the catalyst of a part of inactivation, add the catalyst that a part is fresh simultaneously.This just causes in beds the catalyst that contains different metal and carbon deposit, in reactor, shorter catalyst only has a small amount of metal and carbon deposit the time of staying, thereby there is higher activity, and such catalyst particle can be drawn off due to the violent back-mixing of reactor, thereby cause the waste of catalyst.Catalyst to different level of deactivation is separated, and makes not inactivation or the lighter catalyst recovery of level of deactivation reuse, and can reduce catalyst loss, greatly reduces the cost of use of catalyst.
US5209840 disclose with the air elutriation separation method from useless catalyst particle by the active catalyst separate particles method out.Reactor that will be last from ebullated bed draws off the catalyst of inactivation and sends into steam stripping unit, and washing catalyst is removed the oil on catalyst.Then the catalyst after stripping is sent into to the air elutriation unit, with the Air Fluidized beds made progress with enough speed, it is expanded, thereby by the catalyst of different level of deactivation separately, high activity, oligosaprobic catalyst are on upper strata, and the catalyst of low activity, high pollution is in lower floor.The efficiency that the method is separated is not high, and operates restive.
The catalyst that US5147527 discloses a kind of high metallic pollution is separated into the method for low-metal content, moderate metallic pollution and high tenor and active catalyst by the Magnetic Isolation method.By after the Cracking catalyst stripping drawn off, coke-burning regeneration, send into afterwards a conductive conveyor belt and remove electrostatic charge, then send into the high magnetic region of magnetic intensity gradient, catalyst is separated, enough magnetic field intensities can make catalyst realize separating with certain transfer rate, and the particle of low magnetic enters first container, this part particle high activity, low metal.The particle of high magnetic enters second container, this part particle low activity, high metal.By the high activated catalyst reducing/regenerating, send the reactor recycling back to.But the method need to will just can be separated after all Burning Coke on Catalyst regeneration, the process complexity.
US5171423 discloses a kind of separating technology of FCU catalyst, and the method is cyclone separation method, and the first step is that the FCC catalyst of coking is separated with hydrocarbon raw material, and second step is that the catalyst of coking is separated with catalyst fines.The method can only separating catalyst density and large catalyst and the catalyst fines of particle size differences.
The fluidisation that Canadian Patent CA1159402 is the density variation of utilizing catalyst particle by lighter hydrocarbons or water reclaims and used, contaminated catalyst, this technique be applicable to be processed the catalyst drawn off from fluid bed or ebullated bed, low-density catalyst passes through coke-burning regeneration after removing lighter hydrocarbons, sends reactor back to; Highdensity catalyst, by processing, reclaims the metal of deposition.The method need to be used a large amount of water or lighter hydrocarbons, although can recycle, process is more complicated.
Summary of the invention
The object of the present invention is to provide a kind of method, a kind of separation method of different level of deactivation catalyst is provided.Separate the used boiling bed residual oil hydrogenation catalyst that carbon deposit and sulphur and various metallic pollutions are arranged, high activity, oligosaprobic catalyst are reclaimed, recycle.The inventive method have can carry out continuously, the advantage such as flexible operation.
The separation method of the different level of deactivation catalyst of the present invention comprises following content:
1, remove and draw off the oil on catalyst, make catalyst be free-flowing;
2, the catalyst that separates different level of deactivation, vertical constant speed split tunnel is set, catalyst to be separated is introduced with the arm of oblique downward direction from the middle and upper part of vertical constant speed split tunnel, air is introduced with the arm of oblique top from the bottom of vertical constant speed split tunnel, vertical constant speed split tunnel top exit is communicated with cyclone separator, the material that cyclone separator reclaims is the catalyst that level of deactivation is light, the material that reclaim vertical constant speed split tunnel bottom is the heavy catalyst of level of deactivation, determine the flow velocity of air velocity and catalyst to be separated, make the material reclaimed from cyclone separator account for 5%～85% of catalyst weight to be separated, be preferably 20%～70%.
In the inventive method, vertical constant speed split tunnel is the straight tube structure, according to the scale of device, diameter and height is set, and as the constant speed split tunnel is that internal diameter is 10mm～30mm, is preferably 15mm～25mm, and length is 50mm～1000mm.The constant speed split tunnel can arrange one, also can arrange as required arranged side by side many.
The catalyst that separation method of the present invention separates is the residual oil boiling bed hydrogenation treatment catalyst, boiling bed hydrogenation treatment catalyst due to when operation in complete back-mixing state, cause the level of deactivation difference of online discharge catalyst, can adopt the inventive method to be separated.The catalyst that the residual oil boiling bed hydrogenation treatment catalyst is regular geometry, be preferably spherically, and particle diameter is 0.08mm～1.50mm, is preferably 0.1mm～1.20mm.Catalyst is loaded catalyst, and active metal component Mo, Ni, Co, W even load are at Al
2o
3, TiO
2, on the carrier such as clay.
In the inventive method, it can be this area conventional method that removal draws off the method that catalyst oils, and a kind of concrete grammar is as follows: the catalyst drawn off from each stage reactor of ebullated bed, at first deliver to the catalyst stripping unit, first, with the varsol washing, remove the heavy oil that catalyst surface adheres to.These varsols can be kerosene, naphtha, toluene, pentane etc. and their mixture.Toluene, ethanol, benzinum equal solvent or the mixed solvent for catalyst that then will tentatively wash carry out stripping, thoroughly remove the oil in catalyst pores, and then vacuum drying makes catalyst reach free-pouring state.
In the inventive method, owing between different level of deactivation catalyst, having density contrast, can be separated by the inventive method, the catalyst recovery that level of deactivation is lighter is recycled, by level of deactivation heavier catalyst treatment, reclaim reactive metal.The inventive method is for separating of the density contrast>0.08kg/m of different level of deactivation catalyst
3, be preferably>0.13kg/m
3, level of deactivation weighs the density>0.08kg/m of the density ratio level of deactivation light catalyst of catalyst
3, be preferably>0.13kg/m
3.
In the inventive method, adopt suitable separator, process the catalyst that the boiling bed hydrogenation processing procedure is discharged, can make the catalyst catalyst heavy with level of deactivation that wherein level of deactivation is light effectively separate, separation process is carried out continuously, and lock out operation is flexible, can be as required, set segregation ratio flexibly, obtain the light catalyst of level of deactivation of desired properties.The inventive method can make the catalyst of different level of deactivation be separated, and inactivation or catalyst that level of deactivation is lighter can reclaim to be reused, thereby reduces catalyst loss, reduces the catalyst cost of use.
The specific embodiment
Catalyst after extracting is processed joins in the loading hopper of separator, set as required suitable reinforced, discharging speed and wind speed, the catalyst separation of different level of deactivation is become to the catalyst that density is lower, level of deactivation is lighter and density is higher, level of deactivation is heavy catalyst.Can first be determined by experiment the serviceability of the catalyst that level of deactivation is light, then determine segregation ratio.During operation, it is constant that charging rate and wind speed will keep, to guarantee separating effect.What the constant speed split tunnel referred to is that charging rate and wind speed are constant.
The loading hopper of separator is positioned at the oblique upper of constant speed split tunnel, when material to be separated enters the constant speed split tunnel, air with certain speed from bottom to top passes through, the granule materials of different densities can realize that under different wind friction velocities balance suspends, the density of material be the wind speed that suspends with balance one to one, low density like this particle enters cyclone separation system on top, realizes separating of particle and air, and low density particle just is separated.Particle sedimentation gradually in the constant speed split tunnel that density is large, flow out from the discharging opening of bottom, thereby realize the separation of different densities particle.
Technical essential of the present invention comprises: the one, must carry out the extracting processing before the catalyst separation of different level of deactivation, and guarantee that decaying catalyst can be free-flowing.The 2nd, the catalyst separation charging rate of different level of deactivation will match with wind speed, guarantees the efficiency of separating.
Further describe technical characterictic of the present invention below in conjunction with embodiment, but be not limited to embodiment.
Embodiment 1
Catalyst by toluene and the ethanol different level of deactivation of mixture extracting of 1: 1, catalyst can be flowed freely, take respectively each 20 grams of catalyst of different level of deactivation, the density of the catalyst that level of deactivation is light is 0.68 grams per milliliter, the density of the catalyst that level of deactivation is heavy is 0.90 grams per milliliter, the two is mixed, material is joined in the loading hopper of separator, the catalyst granules that separates this density contrast, the constant speed split tunnel length of selecting is 1000mm, sets charging rate and is separated with wind speed.Take the low density catalyst after separation, weight is 13.8 grams, and separative efficiency is 69.0%.
Embodiment 2
Catalyst by toluene and the ethanol different level of deactivation of mixture extracting of 1: 1, catalyst can be flowed freely, take respectively each 20 grams of catalyst of different level of deactivation, the density of the catalyst that level of deactivation is light is 0.68 grams per milliliter, the density of the catalyst that level of deactivation is heavy is 1.17 grams per milliliters, the two is mixed, material is joined in the loading hopper of separator, the catalyst granules that separates this density contrast, the constant speed split tunnel length of selecting is 200mm, sets charging rate and is separated with wind speed.Take the low density catalyst after separation, weight is 15.2 grams, and separative efficiency is 76.0%.
Embodiment 3
The catalyst of the different level of deactivation that draw off from fluidized bed reactor with toluene and the ethanol mixture extracting of 1: 1, catalyst can be flowed freely, take catalyst 200 grams of different level of deactivation, material is joined in the loading hopper of separator, the constant speed split tunnel length of selecting is 1000mm, sets charging rate and is separated with wind speed, obtains catalyst 75 grams that level of deactivation is light, density is 0.71 grams per milliliter, and the density of the catalyst that the level of deactivation obtained is heavy is 1.02 grams per milliliters.Catalyst after separating is carried out respectively to the coke-burning regeneration processing, and in laboratory, it is carried out to the autoclave evaluation, and corresponding fresh catalyst activity contrasted, be the results are shown in Table 1.
The Hydrogenation of the isolated different densities catalyst of table 1
As seen from the table, being more or less the same of isolated low-density catalyst hydrogenation metal removal activity and hydrodesulfurization activity and fresh dose, can be recycled.
Claims (11)
1. the separation method of different level of deactivation catalyst, comprise following content: remove and draw off the oil on catalyst, make catalyst be free-flowing, the catalyst that separates different level of deactivation, it is characterized in that: vertical constant speed split tunnel is set, catalyst to be separated is introduced with the arm of oblique downward direction from the middle and upper part of vertical constant speed split tunnel, air is introduced with the arm of oblique top from the bottom of vertical constant speed split tunnel, vertical constant speed split tunnel top exit is communicated with cyclone separator, the material that cyclone separator reclaims is the catalyst that level of deactivation is light, the material that reclaim vertical constant speed split tunnel bottom is the heavy catalyst of level of deactivation, determine the flow velocity of air velocity and catalyst to be separated, make the material reclaimed from cyclone separator account for 5%～85% of catalyst weight to be separated.
2. it is characterized in that in accordance with the method for claim 1: make the material reclaimed from cyclone separator account for 20%～70% of catalyst weight to be separated.
3. in accordance with the method for claim 1, it is characterized in that: vertical constant speed split tunnel is the straight tube structure, and the constant speed split tunnel is that internal diameter is 10mm～30mm, and length is 50mm～1000mm.
4. it is characterized in that in accordance with the method for claim 3: the internal diameter that vertical constant speed split tunnel is is 15mm～25mm.
5. in accordance with the method for claim 1, it is characterized in that: the constant speed split tunnel arranges one, or arranges arranged side by side many.
6. in accordance with the method for claim 1, it is characterized in that: catalyst is the residual oil boiling bed hydrogenation treatment catalyst, the catalyst that the residual oil boiling bed hydrogenation treatment catalyst is regular geometry.
7. in accordance with the method for claim 6, it is characterized in that: catalyst is that the residual oil boiling bed hydrogenation treatment catalyst is spherical, and particle diameter is 0.08mm～1.50mm.
8. it is characterized in that in accordance with the method for claim 7: the spherical particle diameters of residual oil boiling bed hydrogenation treatment catalyst is 0.1mm～1.20mm.
9. it is characterized in that in accordance with the method for claim 1: the density>0.08kg/m of the density ratio level of deactivation light catalyst of the heavy catalyst of level of deactivation
3.
10. it is characterized in that in accordance with the method for claim 1: the density>0.13kg/m of the density ratio level of deactivation light catalyst of the heavy catalyst of level of deactivation
3.
11. it is characterized in that in accordance with the method for claim 3: the constant speed split tunnel is that internal diameter is 15mm～25mm.
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| CN104606946B (en) * | 2015-01-09 | 2016-05-11 | 中国天辰工程有限公司 | In a kind of adiponitrile production process, separate the method for inactivation curing catalysts |
| CN106000478A (en) * | 2016-05-19 | 2016-10-12 | 福州大学化肥催化剂国家工程研究中心 | Recycling method of slurry-bed hydrocracking catalyst for heavy oil |
| CN107597201B (en) * | 2017-09-13 | 2019-10-08 | 上海华畅环保设备发展有限公司 | Oil-containing outlet catalyst treatment and sorting reuse method and device |
| CN112439462B (en) * | 2019-09-02 | 2023-05-05 | 中国石油化工股份有限公司 | Method for recycling waste hydrogenation catalyst |
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| CN1528737A (en) * | 2003-10-10 | 2004-09-15 | 清华大学 | Apparatus and method for preparing aminobenzene by nitrobenzene gas-phase hydrogenation |
| CN1864844A (en) * | 2006-04-20 | 2006-11-22 | 四川材料与工艺研究所 | Apparatus and method for hydrogen oxygen composite reaction |
| CN1958146A (en) * | 2006-10-13 | 2007-05-09 | 宜宾天原股份有限公司 | Multiple stage fluidized-bed reactor and method for synthesizing chloroethylene |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1528737A (en) * | 2003-10-10 | 2004-09-15 | 清华大学 | Apparatus and method for preparing aminobenzene by nitrobenzene gas-phase hydrogenation |
| CN1864844A (en) * | 2006-04-20 | 2006-11-22 | 四川材料与工艺研究所 | Apparatus and method for hydrogen oxygen composite reaction |
| CN1958146A (en) * | 2006-10-13 | 2007-05-09 | 宜宾天原股份有限公司 | Multiple stage fluidized-bed reactor and method for synthesizing chloroethylene |
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