CN108212135A - The recycling and processing device and method of dead catalyst in a kind of Bravo synthesis technology - Google Patents

The recycling and processing device and method of dead catalyst in a kind of Bravo synthesis technology Download PDF

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Publication number
CN108212135A
CN108212135A CN201711488814.4A CN201711488814A CN108212135A CN 108212135 A CN108212135 A CN 108212135A CN 201711488814 A CN201711488814 A CN 201711488814A CN 108212135 A CN108212135 A CN 108212135A
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bravo
catalyst
dead catalyst
roasting
unit
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***
王海波
郝德新
禚文峰
庞怀林
谢思勉
田晓宏
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Nantong Taihe Chemical Ltd By Share Ltd
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Nantong Taihe Chemical Ltd By Share Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/18Carbon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/20Regeneration or reactivation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00Regeneration or reactivation of catalysts, in general
    • B01J38/02Heat treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00Regeneration or reactivation of catalysts, in general
    • B01J38/04Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00Regeneration or reactivation of catalysts, in general
    • B01J38/04Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
    • B01J38/12Treating with free oxygen-containing gas
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00Regeneration or reactivation of catalysts, in general
    • B01J38/72Regeneration or reactivation of catalysts, in general including segregation of diverse particles
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C253/00Preparation of carboxylic acid nitriles
    • C07C253/32Separation; Purification; Stabilisation; Use of additives
    • C07C253/34Separation; Purification
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/584Recycling of catalysts

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Catalysts (AREA)

Abstract

The present invention relates to the recycling and processing device and method of dead catalyst in a kind of Bravo synthesis technology, device includes roasting unit and the flue gas trapping unit and regenerating active carbon unit that are attached thereto respectively.Method includes the following steps:(1) after dead catalyst is dehydrated, heating, for the first time roasting removes low-boiling-point substance, continues to heat up, and second of roasting removes high-boiling components;(2) flue gas obtained by trapping step (1), obtains organic detritus;(3) catalyst after collection step (1) processing, screening meet the regenerated activated carbon of conduct of Particle size requirements.The present invention realizes the continuous recycling of waste active carbon catalyst, regenerated activated-carbon catalyst is recycled and reused in Bravo synthesis technology and keeps high activity, Bravo molar yield is more than 85%, and Bravo content is in more than 90wt% in product, while regenerated carbon reaches more than 60wt%;Organic detritus is sold by refining to can obtain Bravo and be used as product.

Description

The recycling and processing device and method of dead catalyst in a kind of Bravo synthesis technology
Technical field
The present invention relates to a kind of times of dead catalyst in pesticide synthesis technical field more particularly to Bravo synthesis technology Receive processing unit and method.
Background technology
Activated carbon is porosity product made of carbonaceous material passes through charing and activation, has very strong adsorptivity.Activity Also there is charcoal physics, chemical property to stablize, acid and alkali-resistance, high temperature resistant, high pressure, not soluble in water and organic solvent, reproducible utilization etc. Plurality of advantages is widely used to the every field such as pharmacy, chemical industry, food and environmental protection.Bravo is killed for substituted benzene broad spectrum activity Epiphyte pharmaceutical, chemical name are 2,4,5,6- tetra- chloro- 1,3- benzene dicarbonitriles (2,4,5,6-tetra chloro-1,3 ,-benzene Dicarbonifrile), belong to less toxic fungicide, there is protective effect.Weak acid, weak base and photo-thermal are stablized, corrosion-free work With.It easily adheres in plant surface, resistance of rainwater washing against, general 7-10 days of the longevity of residure.It is mainly used for fruit tree, rust, anthrax on vegetables The prevention of disease, powdery mildew, downy mildew.Catalyst used in Bravo synthesis is coconut husk class activated carbon, such activated carbon compares table Area is big, and ash content is low, there is good catalytic action in the synthetic reaction of Bravo.Such activated-carbon catalyst is using one After the section time, the high boiling Organic Material Blocking duct of catalyst causes specific surface area to reduce significantly, has seriously affected and urged The absorption property and catalytic performance of agent.
The waste active carbon catalyst inactivated after using is handled in the prior art as hazardous waste, general landfill or It directly burns, due to being adsorbed with the largely organic matter containing chlorine element in dead catalyst micropore, directly landfill can cause environment Certain pollution.Since dead catalyst chlorinity is very high, direct burning disposal can cause solid waste burning equipment to corrode, and cause to set Standby damage, common burning facility is rotary kiln, and such catalyst and organic waste residues cannot all recycle, and is directly destroyed.If The organic matter that can be adsorbed to dead catalyst and dead catalyst detaches, and the two is recycled, that is, solves dangerous waste Handling problems realize the reuse of activated-carbon catalyst again, save cost.
It is developing history longest, a kind of most widely used regeneration method to heat method of reproduction.Heating regenerative process is to utilize The characteristics of adsorbate in adsorption saturation activated carbon can be desorbed from activated carbon gap at high temperature, makes adsorbate in high temperature Lower desorption so as to which the micro cellular voids that activated carbon is made to be blocked originally are opened, restores its absorption property.After applying high temperature, molecule shakes Dynamic kinetic energy increases, and changes its adsorption equilibrium relationship, and binding molecule is made to be detached from activated carbon surface and enters gas phase.Heating regeneration due to Diversified adsorbate can be decomposed and there is versatility, and regeneration is more thorough, is always the mainstream of regeneration method. The shortcomings of heating regeneration has many advantages, such as that regeneration rate is high, and the recovery time is short, but there is also regeneration loss, and operating condition is stringent.And And the regenerated temperature of heating of the prior art is very high, and supplement water is usually also needed to while 700 DEG C or more, high-temperature operation Steam is activated, such as CN104190478A discloses a kind of regeneration side of the cerium modified activated carbon denitration desulphurization catalyst of vanadium Method purges activated carbon including the gaseous mixture containing vapor, if for recycling dangerous waste catalyst, not only to the corruption of equipment Erosion is very serious, is not suitable for the high chlorine dead catalyst generated in Bravo synthesis technology processing, and can not recycle organic detritus In product.CN103288079A needs the activation for adding in vapor at 800-1000 DEG C and carrying out activated carbon, and energy consumption is higher.
Invention content
In view of in Bravo synthesis technology in the prior art dead catalyst as dangerous waste be difficult processing, can not return The problem of receipts, one of the objects of the present invention is to provide a kind of catalyst recycling and processing device and methods, and Bravo can be synthesized Dead catalyst and the organic matter of dead catalyst absorption are detached, and the two is recycled in technique, have both solved danger Useless handling problems realize the reuse of activated-carbon catalyst again, save cost, economize on resources, environmental protection.
The purpose of the present invention is achieved through the following technical solutions:
In a first aspect, the present invention provides a kind of recycling and processing device of dead catalyst in Bravo synthesis technology, including roasting Burn unit and the flue gas trapping unit and regenerating active carbon unit that are attached thereto respectively.
Dead catalyst enters roasting unit and is roasted, and treated, and catalyst is obtained by regenerating active carbon cell processing To regenerated activated-carbon catalyst;The flue gas that roasting unit generates simultaneously by flue gas trapping unit, be caught by the dust in flue gas Collect as organic detritus, which is easy to get Bravo product after refined.
Preferably, the roasting unit includes rotary drum furnace.
Preferably, the roasting unit is heat stepwise structure.
Preferably, the feed inlet of the roasting unit is equipped with hopper, passes through between the bottom of the hopper and roasting unit Conveying device connects.
Preferably, the conveying device includes helix transporting device.
Preferably, the conveying device is equipped with frequency converter, controls the feed flow of dead catalyst.
Preferably, the flue gas trapping unit includes stainless steel trap.
Preferably, the stainless steel trap includes individual layer stainless steel trap or chuck stainless steel trap.
Preferably, outlet pass and/or air inlet are equipped in the chuck of the chuck stainless steel trap.
Preferably, the flue gas trapping unit includes organic residue collector.
Preferably, the gas outlet of the flue gas trapping unit connects organic burned waste gas unit, and organic exhaust gas burns rear molding Gas qualified discharge.
Preferably, the regenerating active carbon unit includes vibrating screen.
Preferably, the vibrating screen includes fine vibrating screen and thick vibrating screen.Can first pass through fine vibrating screen passing through Thick vibrating screen is crossed, can also be inverted.
Preferably, the mesh number of the fine vibrating screen ranging from 60-100 mesh, preferably 70-80 mesh.
Preferably, the mesh number of the thick vibrating screen ranging from 5-10 mesh, preferably 6-8 mesh.
Second aspect, the present invention provides a kind of recovery and treatment method of dead catalyst in Bravo synthesis technology, including such as Lower step:
(1) it roasts:After dead catalyst is put dehydration, heating, for the first time roasting removes low-boiling-point substance, continues to heat up, second Roasting removes high-boiling components;
(2) organic detritus is recycled:The flue gas obtained by step (1) is trapped, obtains organic detritus;
(3) regenerating active carbon:Catalyst after collection step (1) processing, screening meets Particle size requirements, as again Raw activated carbon.
Preferably, step (1) further includes and gas is passed through into the dead catalyst, and the gas includes air, pure nitrogen gas With any one in purity oxygen or at least two combination.
It is passed through gas and crosses and activated-carbon catalyst ontology is at most caused to be aoxidized, destroy catalyst microcellular structure, catalyst returns Yield declines, and activity also can be impacted.Being passed through the organic matter adsorbed in the very few activated-carbon catalyst micropore of gas cannot divide completely Solution, the catalyst activity for causing recycling be not high.Preferably, the volume mass ratio of step (1) gas and the dead catalyst For 1.5-3m3/ kg, such as 1.5m3/kg、1.6m3/kg、 1.8m3/kg、2.0m3/kg、2.1m3/kg、2.2m3/kg、2.3m3/kg Or 2.5m3/ kg etc., preferably 2-2.5m3/kg。
Preferably, the temperature of step (1) described dehydration is 90-140 DEG C.
Preferably, the temperature of step (1) first time roasting is 280-330 DEG C, for example, 280 DEG C, 290 DEG C, 300 DEG C, 310 DEG C, 320 DEG C or 330 DEG C etc.;Time be 1~2.3h, such as 1h, 1.2h, 1.5h, 1.8h, 2.0h, 2.1h, 2.2h or 2.3h etc., preferably 1.5~1.8h.
Preferably, the temperature of step (1) second roasting is 580-630 DEG C, for example, 580 DEG C, 590 DEG C, 600 DEG C, 610 DEG C, 620 DEG C or 630 DEG C etc.;Time be 1~2.5h, such as 1h, 1.2h, 1.3h, 1.5h, 1.6h, 1.7h, 1.8h, 1.9h, 2.0h, 2.1h, 2.3h or 2.5h etc., preferably 1.5~2h.
Preferably, step (2) described organic detritus is refined, and obtains Bravo.Present invention recycling gained organic detritus The content of middle Bravo can be refining to obtain purifying Bravo product in more than 80wt%, by existing separation purifying technique, For selling.
Preferably, the recovery and treatment method of dead catalyst utilizes as described in relation to the first aspect in the Bravo synthesis technology Bravo synthesis technology in dead catalyst recycling and processing device carry out.
Preferably, the recovery and treatment method of dead catalyst includes the following steps in the Bravo synthesis technology:
(1) it roasts:The dead catalyst is continuously introduced into roasting unit, while is continuously passed through the gas, described give up is urged Agent is dehydrated successively, roasting for the first time removes low-boiling-point substance, second of roasting removes high-boiling components;Gas has in the water smoking The effect of vapor in catalyst porous structure is purged, accelerates dry and optimizing drying effect, is prepared for follow-up roasting.
(2) organic detritus is recycled:Flue gas obtained by step (1) enters flue gas trapping unit, obtains organic detritus;
(3) regenerating active carbon:The catalyst that step (1) described roasting unit continuously exports enters regenerating active carbon unit, Screening meets Particle size requirements, as the regenerated activated carbon.
Preferably, preceding 1/3rd sections of temperature for setting the calciner are 90-140 DEG C, intermediate 1/3rd sections of temperature It is 280-330 DEG C to spend, and rear 1/3rd sections of temperature are 580-630 DEG C;
Roasting time is long, and activated carbon ontology is caused to be aoxidized, and roasting time deficiency causes activated-carbon catalyst micropore The organic matter of interior absorption cannot decompose completely, and the catalyst activity after recycling is not high.Preferably, the dead catalyst is described In calciner the residence time be 2-5h, such as 2h, 2.2h, 2.3h, 2.5h, 2.8h, 3h, 3.2h, 3.5h, 3.8h, 4h, 4.5h or 5h etc., preferably 3-4h.
The present invention coordinates with roasting time by the volume mass of gas and dead catalyst ratio, ensures the catalysis after recycling The activity of agent, and ensure the content of Bravo and the rate of recovery of regenerated catalyst in gained organic detritus simultaneously.
Compared with prior art, the present invention at least has the advantages that:
With in the prior art using dead catalyst in Bravo synthesis technology compared with the conventional treatment thinking of dangerous waste, this New diameter is separately warded off in invention, will set flue gas trapping unit and regenerating active carbon unit after roasting unit respectively, realizes useless activity Pd/carbon catalyst is continuously recycled production, and regenerated activated-carbon catalyst is recycled and reused in Bravo synthesis technology and keeps high Activity, Bravo molar yield is more than 85%, and the content of Bravo is in more than 90wt% in product, while regenerated carbon The rate of recovery reaches more than 60wt%;The organic detritus of roasting out is sold by refining to be easy to get Bravo and be used as product.Section Cost-saving economizes on resources, environmental protection.
Description of the drawings
Fig. 1 is the retracting device schematic diagram that the embodiment of the present invention 1 is used to produce the catalyst of Bravo;
Fig. 2 is the recovery processing technique flow chart of dead catalyst in 1 Bravo synthesis technology of the embodiment of the present invention.
The mark in the figure shows:1- helix transporting devices, 2- hoppers, 3- rotary drum furnaces, 4- traps, 5- tail gas burn dress It puts, the thick vibrating screens of 6-, the fine vibrating screens of 7-
Specific embodiment
Technical solution to further illustrate the present invention below with reference to the accompanying drawings and specific embodiments.It is but following Example is only the simple example of the present invention, does not represent or limit the scope of the present invention, protection model of the invention It encloses and is subject to claims.
Embodiment 1
The recycling and processing device of dead catalyst in a kind of Bravo synthesis technology, as shown in Figure 1, including heat stepwise knot Rotary drum furnace 3, trap 4, fine vibrating screen 7, thick vibrating screen 6 and the tail gas incinerator 5 of structure.
Wherein, the feed inlet of rotary drum furnace 3 is equipped with hopper 2, is equipped between the bottom of hopper 2 and rotary drum furnace 3 for continuous The helix transporting device 1 of charging adjusts conveying capacity by frequency converter, and hopper 2 and bolt conveying device 1 are stainless steel 304 material Matter.3 furnace body material of rotary drum furnace is stainless steel 304, and 4 material of trap is Stainless steel 316 L, is individual layer trap not jacketed. The material of fine vibrating screen 7 and thick vibrating screen 6 is stainless steel 304, and tail gas incinerator 5 is complete modular system.
The recovery processing technique of dead catalyst in Bravo synthesis technology is carried out using above device, as shown in Fig. 2, step It is rapid as follows:
(1) it roasts:/ 3rd sections of temperature are 100 DEG C before setting rotary drum furnace 3, and intermediate 1/3rd sections of temperature are 300 DEG C, rear 1/3rd sections of temperature are 600 DEG C, are continuously introduced into dead catalyst thereto, while be continuously passed through air, are passed through gas Total amount (m3/ h) with dead catalyst enter rotary drum furnace 3 quality (kg/h) ratio be 2:1, dead catalyst stops in rotary drum furnace 3 Time is 3h, is dehydrated successively, roasting for the first time removes low-boiling-point substance, second of roasting removes high-boiling components;
(2) organic detritus is recycled:Flue gas obtained by step (1) enters trap 4, obtains organic detritus, refines out hundred bacterium Clearly;
(3) regenerating active carbon:The catalyst that step (1) rotary drum furnace 3 continuously exports enters the fine vibrating screen 7 of 80 purposes again Into the thick vibrating screen 6 of 6 purposes, regenerated activated carbon is filtered out.
The technique solves the problems, such as the disposition of Bravo waste catalyst recovery.Waste active carbon catalyst is realized continuously to return Process for producing, activated-carbon catalyst recycling are received, the organic detritus for roasting out can refine out Bravo as product pin It sells.Cost is saved, is economized on resources, environmental protection.Embodiment activated-carbon catalyst rate of recovery 70wt%, the activity after regeneration Pd/carbon catalyst is used for the molar yield 93.6% of Bravo production, and the content of Bravo reaches 98.5wt% in product.
Embodiment 2
With differing only in for embodiment 1:It is passed through gas and replaces with pure nitrogen gas.
Embodiment activated-carbon catalyst rate of recovery 81wt%, the activated-carbon catalyst after recycling produce for Bravo Molar yield 81.8%, the content 91.3wt% of Bravo in product.
Embodiment 3
With differing only in for embodiment 1:It is 1 to be passed through gas and replace with volume ratio:The mixing of 1 pure nitrogen gas and air Gas.
Embodiment activated-carbon catalyst rate of recovery 76wt%, the activated-carbon catalyst after recycling produce for Bravo Molar yield 88.5%, the content 95.8wt% of Bravo in product.
Embodiment 4
With embodiment 1 difference lies in:Dead catalyst is 4h in roller residing time in furnace, is passed through air total amount (m3/ H) quality (kg/h) ratio for entering rotary drum furnace with dead catalyst is 1.5:1.
Embodiment activated-carbon catalyst rate of recovery 67wt%, the activated-carbon catalyst after recycling produce for Bravo Molar yield 93.8%, the content 98.2wt% of Bravo in product.
Embodiment 5
With embodiment 1 difference lies in:/ 3rd sections of temperature are 90 DEG C before rotary drum furnace, intermediate 1/3rd sections of temperature It it is 290 DEG C, rear 1/3rd sections of temperature are 580 DEG C;It is 1 to be passed through gas and replace with volume ratio:1 pure nitrogen gas and air it is mixed Close gas.
Embodiment activated-carbon catalyst rate of recovery 82wt%, the activated-carbon catalyst after recycling produce for Bravo Molar yield 85.5%, the content 93.1wt% of Bravo in product.
Embodiment 6
With embodiment 1 difference lies in:/ 3rd sections of temperature are 140 DEG C before rotary drum furnace, intermediate 1/3rd sections of temperature It it is 330 DEG C, rear 1/3rd sections of temperature are 630 DEG C;It is 1 to be passed through gas and replace with volume ratio:1 pure nitrogen gas and air it is mixed Close gas.
Embodiment activated-carbon catalyst rate of recovery 67wt%, the activated-carbon catalyst after recycling produce for Bravo Molar yield 85.5%, the content 98.3wt% of Bravo in product.
Embodiment 7
With differing only in for embodiment 1:It is passed through air total amount (m3/ h) with dead catalyst enter the quality of rotary drum furnace (kg/h) ratio is 1.5:1.
Embodiment activated-carbon catalyst rate of recovery 75wt%, the activated-carbon catalyst after recycling produce for Bravo Molar yield 92.2%, the content of Bravo reaches 97.9wt% in product.
Embodiment 8
With differing only in for embodiment 1:It is 2 to be passed through gas and replace with volume ratio:The mixing of 1 pure nitrogen gas and air Gas.
Embodiment activated-carbon catalyst rate of recovery 79wt%, the activated-carbon catalyst after recycling produce for Bravo Molar yield 87.6%, the content 95.2wt% of Bravo in product.
Embodiment 9
With embodiment 1 difference lies in:It is 3 to be passed through gas and replace with volume ratio:1 pure nitrogen gas and the gaseous mixture of air, It is passed through gas gross (m3/ h) with dead catalyst enter rotary drum furnace quality (kg/h) ratio be 3:1, dead catalyst is in rotary drum furnace The interior residence time is 5h, and the mesh number of fine vibrating screen is 100 mesh, and the mesh number of thick vibrating screen is 10 mesh.
Embodiment activated-carbon catalyst rate of recovery 62wt%, the activated-carbon catalyst after recycling produce for Bravo Molar yield 87.8%, the content 94.7wt% of Bravo in product.
Embodiment 10
With embodiment 1 difference lies in:It is 1 to be passed through gas and replace with volume ratio:2 pure nitrogen gas and the gaseous mixture of air, It is passed through gas gross (m3/ h) with dead catalyst enter rotary drum furnace quality (kg/h) ratio be 2.5:1, dead catalyst is in roller Residing time in furnace is 2h, and the mesh number of fine vibrating screen is 70 mesh, and the mesh number of thick vibrating screen is 5 mesh.
Embodiment activated-carbon catalyst rate of recovery 75wt%, the activated-carbon catalyst after recycling produce for Bravo Molar yield 85.8%, the content 92.5wt% of Bravo in product.
Embodiment 11
With embodiment 1 difference lies in:It is passed through gas gross (m3/ h) with dead catalyst enter the quality (kg/ of rotary drum furnace H) ratio is 3.5:1.
Embodiment activated-carbon catalyst rate of recovery 66wt%, the activated-carbon catalyst after recycling produce for Bravo Molar yield 85.2%, the content 90.6wt% of Bravo in product.
Embodiment 12
With embodiment 1 difference lies in:It is passed through gas gross (m3/ h) with dead catalyst enter the quality (kg/ of rotary drum furnace H) ratio is 1:1.
Embodiment activated-carbon catalyst rate of recovery 80wt%, the activated-carbon catalyst after recycling produce for Bravo Molar yield 83.5%, the content 90.8wt% of Bravo in product.
Embodiment 13
With embodiment 1 difference lies in:Dead catalyst is 5.5h in roller residing time in furnace.
Embodiment activated-carbon catalyst rate of recovery 66wt%, the activated-carbon catalyst after recycling produce for Bravo Molar yield 86.3%, the content 91.2wt% of Bravo in product.
Embodiment 14
With embodiment 1 difference lies in:Dead catalyst is 1h in roller residing time in furnace.
Embodiment activated-carbon catalyst rate of recovery 79wt%, the activated-carbon catalyst after recycling produce for Bravo Molar yield 86.8%, the content 90.5wt% of Bravo in product.
In addition, the regeneration activity of embodiment 11 and embodiment 13 follow-up refined compared to 1 gained Bravo of embodiment The Pd/carbon catalyst rate of recovery, Bravo quality are decreased obviously.Total organic detritus amount is insufficient obtained by embodiment 12 and embodiment 14, The rate of recovery of Bravo declines therewith in organic detritus, and the activated-carbon catalyst activity after recycling is not also high.Integrated comparative is implemented Example 1 is with embodiment 11~14 it is found that the present invention is by the volume mass of gas and dead catalyst ratio, with roasting time phase interworking It closes, optimizes the activity of catalyst, and ensure that the recycling of the rate of recovery, recycling quality and regenerated catalyst of Bravo is received simultaneously Rate.
Applicant states that the present invention illustrates the detailed process equipment of the present invention and technological process by above-described embodiment, But the invention is not limited in above-mentioned detailed process equipment and technological processes, that is, it is above-mentioned detailed not mean that the present invention has to rely on Thin process equipment and technological process could be implemented.Person of ordinary skill in the field is it will be clearly understood that change any of the present invention Into the addition of equivalence replacement and auxiliary element to each raw material of product of the present invention, selection of concrete mode etc. all fall within this hair Within bright protection domain and the open scope.

Claims (10)

1. the recycling and processing device of dead catalyst in a kind of Bravo synthesis technology, which is characterized in that including roasting unit and divide The flue gas trapping unit and regenerating active carbon unit not connect with the roasting unit.
2. the recycling and processing device of dead catalyst in Bravo synthesis technology as described in claim 1, which is characterized in that described Roasting unit includes rotary drum furnace;
Preferably, the roasting unit is heat stepwise structure.
3. the recycling and processing device of dead catalyst in Bravo synthesis technology as claimed in claim 1 or 2, which is characterized in that The feed inlet of the roasting unit is equipped with hopper, is connected between the bottom of the hopper and roasting unit by conveying device;
Preferably, the conveying device includes helix transporting device;
Preferably, the conveying device is equipped with frequency converter.
4. such as the recycling and processing device of dead catalyst in claim 1-3 any one of them Bravo synthesis technologies, feature It is, the flue gas trapping unit includes stainless steel trap;
Preferably, the stainless steel trap includes individual layer stainless steel trap or chuck stainless steel trap;
Preferably, outlet pass and/or air inlet are equipped in the chuck of the chuck stainless steel trap.
5. such as the recycling and processing device of dead catalyst in claim 1-4 any one of them Bravo synthesis technologies, feature It is, the flue gas trapping unit includes organic residue collector;
Preferably, the gas outlet of the flue gas trapping unit connects organic burned waste gas unit.
6. such as the recycling and processing device of dead catalyst in claim 1-5 any one of them Bravo synthesis technologies, feature It is, the regenerating active carbon unit includes vibrating screen;
Preferably, the vibrating screen includes fine vibrating screen and thick vibrating screen;
Preferably, the mesh number of the fine vibrating screen ranging from 60-100 mesh, preferably 70-80 mesh;
Preferably, the mesh number of the thick vibrating screen ranging from 5-10 mesh, preferably 6-8 mesh.
7. the recovery and treatment method of dead catalyst in a kind of Bravo synthesis technology, which is characterized in that include the following steps:
(1) it roasts:After dead catalyst is dehydrated, heating, for the first time roasting removes low-boiling-point substance, continues to heat up, and second of roasting removes Remove high-boiling components;
(2) organic detritus is recycled:The flue gas obtained by step (1) is trapped, obtains organic detritus;
(3) regenerating active carbon:Catalyst after collection step (1) processing, screening meets Particle size requirements, as regenerated work Property charcoal.
8. the recovery and treatment method of dead catalyst in Bravo synthesis technology as claimed in claim 7, which is characterized in that step (1) it further includes and gas is passed through into the dead catalyst, the gas includes any one in air, pure nitrogen gas and purity oxygen Or at least two combination;
Preferably, the volume mass ratio of the gas and the dead catalyst is 1.5-3m3/ kg, preferably 2-2.5m3/kg;
Preferably, the temperature of step (1) described dehydration is 90-140 DEG C;
Preferably, the temperature of step (1) first time roasting is 280-330 DEG C, and the time is 1~2.3h, preferably 1.5~ 1.8h;
Preferably, the temperature of step (1) second of roasting is 580-630 DEG C, and the time is 1~2.5h, preferably 1.5~2h;
Preferably, step (2) described organic detritus is refined, and obtains Bravo.
9. the recovery and treatment method of dead catalyst in Bravo synthesis technology as claimed in claim 7 or 8, which is characterized in that The recovery and treatment method of dead catalyst utilizes such as claim 1-6 any one of them Bravos in the Bravo synthesis technology The recycling and processing device of dead catalyst carries out in synthesis technology.
10. the recovery and treatment method of dead catalyst in Bravo synthesis technology as claimed in claim 9, which is characterized in that institute The recovery and treatment method for stating dead catalyst in Bravo synthesis technology includes the following steps:
(1) it roasts:The dead catalyst is continuously introduced into roasting unit, while is continuously passed through the gas, the dead catalyst It is dehydrated successively, roasting for the first time removes low-boiling-point substance, second of roasting removes high-boiling components;
(2) organic detritus is recycled:Flue gas obtained by step (1) enters flue gas trapping unit, obtains organic detritus;
(3) regenerating active carbon:The catalyst that step (1) described roasting unit continuously exports enters regenerating active carbon unit, screening Meet Particle size requirements, as the regenerated activated carbon;
Preferably, preceding 1/3rd sections of temperature for setting the calciner are 90-140 DEG C, and intermediate 1/3rd sections of temperature are 280-330 DEG C, rear 1/3rd sections of temperature are 580-630 DEG C;
Preferably, dead catalyst residence time in the calciner is 2-5h, preferably 3-4h.
CN201711488814.4A 2017-12-29 2017-12-29 The recycling and processing device and method of dead catalyst in a kind of Bravo synthesis technology Pending CN108212135A (en)

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