CN104307479A - Regeneration method of invalid carbon molecular sieve - Google Patents
Regeneration method of invalid carbon molecular sieve Download PDFInfo
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- CN104307479A CN104307479A CN201410621163.1A CN201410621163A CN104307479A CN 104307479 A CN104307479 A CN 104307479A CN 201410621163 A CN201410621163 A CN 201410621163A CN 104307479 A CN104307479 A CN 104307479A
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- molecular sieve
- carbon molecular
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- regeneration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3483—Regenerating or reactivating by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/42—Materials comprising a mixture of inorganic materials
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- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Separation Of Gases By Adsorption (AREA)
Abstract
The invention relates to a regeneration method of an invalid carbon molecular sieve. The regeneration method comprises the following steps: firstly, placing the failure carbon molecular sieve in a carbon molecular sieve regeneration treatment furnace, rotating a furnace pipe at the speed of 10-15 turn/minute, rising the temperature to 280 DEG C, and keeping the temperature; then, feeding carbonized tail gas produced by a carbon molecular sieve thermal treatment furnace which is performing carbonizing treatment into the carbon molecular sieve regeneration treatment furnace in which the failure carbon molecular sieve is placed, and feeding the carbonized tail gas for 30 to 60 minutes after rising the carbonizing temperature to 400 DEG C; obtaining a regenerated carbon molecular sieve after cooling, wherein, the thermal treatment furnace which produces carbonized tail gas and the carbon molecular sieve regeneration treatment furnace are the same in specification, and the regenerated carbon molecular sieve can reach the indexes before invalidation. The regeneration method has the advantages of simple technology, low cost, energy conservation, consumption reduction, low pollution and high production efficiency.
Description
Technical field
The present invention relates to technical field of molecular sieve, particularly a kind of renovation process of the carbon molecular sieve that lost efficacy.
Background technology
Carbon molecular sieve is adsorbent special in a kind of THE PRESSURE SWING ADSORPTION NITROGEN GENERATING DEVICE, is widely used in nitrogen industry processed, its special micropore (aperture 0.3nm ~ 0.5nm), is very beneficial for being separated N
2, O
2.
Just because of the aperture structure that carbon molecular sieve is too small, it in use if air-source process is not up to standard, very easily causes carbon molecular sieve blockage of the micro orifice, causes separating effect to decline, thus is formed " inefficacy " of carbon molecular sieve, also referred to as " poisoning ".
For the carbon molecular sieve lost efficacy, do not have good method at present, most employing waste treatment, has individually process such as adopting pickling, washing, charing, activation, tune hole.Such as, Chinese patent application 2012103019373 discloses a kind of renovation process of nitrogen-preparing carbon molecular sieves, comprises the steps such as pickling, washing, carbonization, activation, tune hole.Achieve under the prerequisite that this renovation process makes carbon molecular sieve not decline at Performance and quality and reuse.Chinese patent application 201310234329X also discloses a kind of renovation process of nitrogen-preparing carbon molecular sieves, and step comprises: screening cleaning: screened through mesh screen by poisoning carbon molecular sieve, then rinses screening the carbon molecular sieve water obtained, and removes impurity; Nitrogen base high temperature carbonization: the carbon molecular sieve cleaned is placed in flue, is warming up to 850-1000 DEG C under nitrogen protection and carbonizes; Mist activates: after high temperature cabonization, pass into CO2, CO mist in flue, wherein CO2 ratio is 85%-90%, and activate the carbon molecular sieve of charing, in-furnace temperature is 700-800 DEG C; Carbon deposition: the carbon molecular sieve after activated is placed in converter flue; converter temperature is 800-900 DEG C; pass into dimethylbenzene under nitrogen protection; keep furnace temperature at 300-500 DEG C, make carbon molecular sieve adsorb dimethylbenzene; then at 800-900 DEG C, dimethylbenzene cracking is made; thus by pyrocarbon on Carbon Materials, aperture adjustment is carried out to carbon molecular sieve, obtains recycled product.Above-mentioned two kinds of renovation process are similar, except pickling and water wash procedures, are substantially repeated the production process of carbon molecular sieve, and whole process is complicated, cost is high, weak effect, and produces secondary pollution.Therefore, its actual application value is also little.
Summary of the invention
Technical problem to be solved by this invention overcomes above-mentioned the deficiencies in the prior art, and provide a kind of simple for process, cost is low, pollution-free, the renovation process of the inefficacy carbon molecular sieve that efficiency is high.
The technical scheme that the present invention solves the problems of the technologies described above employing is: a kind of renovation process of the carbon molecular sieve that lost efficacy, is characterized in that comprising the following steps:
(1) first loaded by inefficacy carbon molecular sieve in carbon molecular sieve regeneration process stove, flue rotates and maintains 10-15 rev/min, is warming up to 280 DEG C, and constant temperature keeps;
(2) then the charing tail gas of the carbon molecular sieve heat-treatment furnace generation carbonizing process will be carried out, passing into the carbon molecular sieve regeneration that inefficacy carbon molecular sieve is housed processes in stove, described charing tail gas rises to after 400 DEG C at heat-treatment furnace carbonization temperature, and the time of passing into is 30-60 minute; The carbon molecular sieve regenerated can be obtained after cooling.
Further, to regenerate the specification processing stove identical for described heat-treatment furnace and the carbon molecular sieve producing charing tail gas.
Further, the described heat-treatment furnace carbonization temperature charing tail gas risen to after 400 DEG C passes into the time in carbon molecular sieve regeneration process stove is 1 hour.
The present invention adopts technique scheme, and the charing tail gas utilizing carbon molecular sieve normally to produce to produce in carbonization process carries out the regeneration of inefficacy carbon molecular sieve under certain temperature conditions.Against existing technologies, its technique of the present invention is simple, and cost is low, and energy-saving and cost-reducing, pollute little, production efficiency is high.Decrease the wasting of resources, alleviate environmental pollution; Regenerative process does not need nitrogen protection.Need not the process such as pickling, washing, charing, activation.Index before institute's regenerative carbon molecular sieve all can reach and lose efficacy.It is a kind of renovation process of desirable inefficacy carbon molecular sieve.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Lost efficacy the renovation process of carbon molecular sieve, and it comprises the following steps:
(1) first loaded by inefficacy carbon molecular sieve in carbon molecular sieve regeneration process stove, flue rotates and maintains 10-15 rev/min, is warming up to 280 DEG C, and constant temperature keeps, stand-by.Current domestic conventional carbon molecular sieve process stove selected by described carbon molecular sieve regeneration process stove, and it is the rotating heat treatment furnace of diameter 350-850mm.Temperature controls at 280 DEG C, and flue rotates and maintains 10-15 rev/min, is conducive to the regeneration of inefficacy carbon molecular sieve.
(2) then by the charing tail gas that the carbon molecular sieve heat-treatment furnace carrying out carbonizing process produces, pass into the carbon molecular sieve regeneration that inefficacy carbon molecular sieve is housed and process in stove.Described charing tail gas rises to after 400 DEG C at heat-treatment furnace carbonization temperature, and the time of passing into is 30-60 minute; The carbon molecular sieve regenerated can be obtained after cooling.After testing, regenerative carbon molecular sieve all can reach the front index that lost efficacy.And carry out a point class wrapper according to index, obtain qualified carbon molecular sieve product.
The charing tail gas that the present invention discharges by collecting heat-treatment furnace charing process, regenerates the carbon molecular sieve lost efficacy.The charing processing procedure normally preparing carbon molecular sieve is: carry out charing process with carbon molecular sieve heat-treatment furnace; heat up under nitrogen protection condition, under described nitrogen protection condition, temperature-rise period nitrogen gas purity used is 95%, flow is 1 ~ 3ml/min, pressure is 0.2Mpa.Temperature-rise period, in 0 ~ 200 DEG C of interval, controls temperature rise rate 5 DEG C/min, in 200 ~ 600 DEG C of intervals, controls temperature rise rate at 15 DEG C/min.In heat-treatment furnace, realize carbon molecular sieve pore-forming, adjust hole process and micropore adjustment.The present invention is by great many of experiments analysis verification, determine to carbon molecular sieve regeneration process stove in pass into charing tail gas opportunity be: normally prepare carbon molecular sieve heat-treatment furnace carbonization temperature rise to 400 DEG C time, now, charing tail gas aqueous two is few, is conducive to the regeneration of inefficacy carbon molecular sieve.
Further, to regenerate the specification processing stove identical for heat-treatment furnace and the carbon molecular sieve producing charing tail gas of the present invention.
Further, the described heat-treatment furnace carbonization temperature charing tail gas risen to after 400 DEG C passes into the time in carbon molecular sieve regeneration process stove is 1 hour.
The charing tail gas that the present invention discharges by collecting heat-treatment furnace charing process, regenerates the carbon molecular sieve lost efficacy.Its technique is simple, and cost is low, and energy-saving and cost-reducing, pollute little, production efficiency is high.Decrease the wasting of resources, alleviate environmental pollution; Regenerative process does not need nitrogen protection.Need not the process such as pickling, washing, charing, activation.Index before institute's regenerative carbon molecular sieve all can reach and lose efficacy.
Embodiment 1: the CMS-220 type that lost efficacy by 100kg carbon molecular sieve loads in the carbon molecular sieve regeneration process stove of diameter 750mm, heats to 280 DEG C of constant temperature, flue rotating speed 10-15 rev/min; In the carbon molecular sieve regeneration process stove of the charing tail gas access dress inefficacy molecular sieve that the carbon molecular sieve heat-treatment furnace being 750mm by the diameter doing charing process produces.Passing into charing tail gas is heat-treatment furnace carbonization temperature when reaching 400 DEG C opportunity, terminates, can obtain regenerating qualified carbon molecule after cooling after continuing to pass into 1 hour.Through inspection, inefficacy carbon molecular sieve recovers original index completely.
Embodiment 2: loaded by inefficacy CMS-240 type carbon molecular sieve 60kg in the carbon molecular sieve regeneration process stove of diameter 500mm, heats to 280 DEG C of constant temperature, flue rotating speed 10-15 rev/min; Select carrying out carbonizing the carbon molecular sieve heat-treatment furnace that the diameter processed is 500mm, passed into by the charing tail gas that heat-treatment furnace produces in the carbon molecular sieves regeneration process stove of inefficacy molecular sieve when temperature reaches 400 DEG C, the time of passing into is after 45 minutes.Then cooling can obtain recycled product naturally.Through inspection, the index of all recycled products all reaches CMS-240 type carbon molecular sieve index.
Embodiment 3: the CMS-260 type carbon molecular sieve 100kg lost efficacy is loaded in carbon molecular sieve regeneration process stove, be warming up to 280 DEG C of constant temperature, flue rotating speed is adjusted to 10-15 rev/min, select same specification carrying out the heat-treatment furnace of the charing process of carbon molecular sieve simultaneously, when heat-treatment furnace carbonization temperature rises to 400 DEG C, the charing tail gas produced passes into the carbon molecular sieve regeneration that inefficacy molecular sieve is housed and processes in stove, and passing into the tail gas time is 30 minutes.Can obtain qualified finished product after cooling, after testing, all indexs all can reach CMS-260 type carbon molecular sieve level to finished product.
Claims (3)
1. lost efficacy the renovation process of carbon molecular sieve, it is characterized in that comprising the following steps:
(1) first loaded by inefficacy carbon molecular sieve in carbon molecular sieve regeneration process stove, flue rotates and maintains 10-15 rev/min, is warming up to 280 DEG C, and constant temperature keeps;
(2) then the charing tail gas of the carbon molecular sieve heat-treatment furnace generation carbonizing process will be carried out, passing into the carbon molecular sieve regeneration that inefficacy carbon molecular sieve is housed processes in stove, described charing tail gas rises to after 400 DEG C at heat-treatment furnace carbonization temperature, and the time of passing into is 30-60 minute; The carbon molecular sieve regenerated can be obtained after cooling.
2. lost efficacy the renovation process of carbon molecular sieve according to claim 1, it is characterized in that: described produce charing tail gas heat-treatment furnace and carbon molecular sieve to regenerate the specification processing stove identical.
3. lost efficacy the renovation process of carbon molecular sieve according to claim 1, it is characterized in that: the time that the described heat-treatment furnace carbonization temperature charing tail gas risen to after 400 DEG C passes in carbon molecular sieve regeneration process stove is 1 hour.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105944674A (en) * | 2016-06-17 | 2016-09-21 | 湖州南浔展辉分子筛厂 | Regeneration method of poisoned carbon molecular sieve |
| CN106915743A (en) * | 2017-01-25 | 2017-07-04 | 威海益正机电科技有限公司 | A kind of preparation method of activated carbon |
Citations (5)
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| US5087778A (en) * | 1990-04-10 | 1992-02-11 | Allied-Signal Inc. | Regeneration of zeolites used for purifying 1,1,1,2-tetrafluoroethane |
| CN101708469A (en) * | 2009-10-27 | 2010-05-19 | 湖州强马分子筛有限公司 | Process for activating and regenerating nitrogen-preparing carbon molecular sieves |
| CN102633253A (en) * | 2012-05-04 | 2012-08-15 | 威海华泰分子筛有限公司 | Method for preparing carbon molecular sieve |
| CN102784631A (en) * | 2012-08-23 | 2012-11-21 | 长兴山立化工材料科技有限公司 | Method for regenerating carbon molecular sieve |
| CN103349973A (en) * | 2013-06-14 | 2013-10-16 | 湖州新奥利吸附材料有限公司 | Regeneration method of nitrogen-preparation carbon molecular sieve |
-
2014
- 2014-11-07 CN CN201410621163.1A patent/CN104307479B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5087778A (en) * | 1990-04-10 | 1992-02-11 | Allied-Signal Inc. | Regeneration of zeolites used for purifying 1,1,1,2-tetrafluoroethane |
| CN101708469A (en) * | 2009-10-27 | 2010-05-19 | 湖州强马分子筛有限公司 | Process for activating and regenerating nitrogen-preparing carbon molecular sieves |
| CN102633253A (en) * | 2012-05-04 | 2012-08-15 | 威海华泰分子筛有限公司 | Method for preparing carbon molecular sieve |
| CN102784631A (en) * | 2012-08-23 | 2012-11-21 | 长兴山立化工材料科技有限公司 | Method for regenerating carbon molecular sieve |
| CN103349973A (en) * | 2013-06-14 | 2013-10-16 | 湖州新奥利吸附材料有限公司 | Regeneration method of nitrogen-preparation carbon molecular sieve |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105944674A (en) * | 2016-06-17 | 2016-09-21 | 湖州南浔展辉分子筛厂 | Regeneration method of poisoned carbon molecular sieve |
| CN106915743A (en) * | 2017-01-25 | 2017-07-04 | 威海益正机电科技有限公司 | A kind of preparation method of activated carbon |
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| CN104307479B (en) | 2016-04-20 |
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