CN1102418C - Regeneration method of waste gas adsorbing and treating system - Google Patents
Regeneration method of waste gas adsorbing and treating system Download PDFInfo
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- CN1102418C CN1102418C CN99109003A CN99109003A CN1102418C CN 1102418 C CN1102418 C CN 1102418C CN 99109003 A CN99109003 A CN 99109003A CN 99109003 A CN99109003 A CN 99109003A CN 1102418 C CN1102418 C CN 1102418C
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Abstract
The present invention relates to a regeneration method of a waste gas adsorbing and treating system. Water and(or) solvent mixture are(is) used for dissolving or washing high-boiling-point organic substances, polymers and dust which are deposited on the surfaces of adsorption agents or in the adsorption agents by an on-line continuous cleaning or extraction method; the used solvents comprise water, ketone and alcohol, one or the mixture of at least two kinds of the solvents are used for regenerating the adsorption agents whose adsorption capacity is degraded at the temperature of 20 DEG C to 80 DEG C in a soaking or a sprinkling mode; the method of the present invention is suitable for a rotating wheel concentration system which uses zeolite or active carbon as an adsorption agent, a fluidized bed adsorption system and a stationary bed adsorption system.
Description
The present invention is a kind of with solvent clean or extraction, with block height in adsorbent surface or duct boil organic matter, polymer or dust etc. with line on continuation mode remove so that adsorbent recovers the renovation process of the waste gas adsorbing and treating system of adsorption capacity.
Absorption method is a kind of method that is widely used on the industry as pump-down process, utilize the character of adsorbent porous, the absorption that VOC, stink or poisonous gas in the industry exhaust can be produced physics or chemistry, and it is adsorbed in the hole of adsorbent, to reach the purpose of purification industry exhaust.Yet adsorbent must be via the program of regeneration after absorption is saturated, with filling in adsorbent be adsorbed matter (for example volatile organic molecule, higher boiling chemical substance ..., etc.) remove, just reusable.The method of at present industrial the most normal employing can be divided into regeneration or two kinds of methods of the outer regeneration of line on the line, regeneration normally utilizes steam or the inert gas that increases temperature will be adsorbed in intrapore organic molecule and displace on the line, for example the clear 63-232823 of day disclosure announcement is taken off the method for absorption with steam (110-175 ℃), will be adsorbed in the interior organic molecule of activated carbon and deviate from the steam method of replacement.BP Brii.1 and for example, 546,437 and 2,419, No. 827 announcements of Deutsche Bundespatent Ger.Offen with high temperature (120-300 ℃) inert gas, the matter that is adsorbed that is adsorbed in the activated carbon is blown down; The clear 63-310636 of the day disclosure then instructs to add hot-air will be adsorbed in the method that the organic substance in the zeolite runner is removed.But the benefit of regenerating on the line is continued operation, and can avoid numerous and diverse adsorbent cargo handling process.Only this kind regeneration is for high boiling chemical substance for example N-methyl-pyrrole noise made in coughing or vomiting ketone (N-MethvlPyrrolidone), methyl-sulfoxide (Dimeihyl Sulfoxide); Monoethanolamine (2-Aminoethanol); Ethylene glycol (Ethylene glycol) then often can't effectively remove, and causes in its hole that residues in adsorbent or decomposes or aggregate into oligomer and influence the ability that adsorbent adsorbs again; In addition if any labile chemicals such as tetramethyl two silicon ammoniums (HMDS), trimethyl silane chance steam such as (Trimethylsilanol) then is decomposed into the solid of silicon hydroxide, residue in the surface of adsorbent and cause the adsorption capacity of adsorbent to descend gradually and the industry exhaust effectively can't be handled to the discharge standard of environmental regulation regulation, have the replacing adsorbent this moment only, or with adsorbent by withdrawing from the adsorption tank, adopt that line is outer directly to be heated or with high temperature oxygen-containing gas (steam for example with high temperature (being generally 300-1000 ℃) more, carbon monoxide or oxygen ..., Deng) handle, to be stranded in the intrapore high-boiling components matter of adsorbent or polymer burn off or decomposition, United States Patent (USP) U.S.4 for example, 957,721; The method that day disclosure special permission 62-282639 and 63-156542... etc. are disclosed.Though this kind method can be adsorbed matter and effectively decomposes and remove being stranded in the intrapore higher boiling of adsorbent, often easily cause the destruction of adsorbent pore space structure and lose adsorption capacity predetermined substance, or thereby deterioration pulverize and lose.The cargo handling process of this external adsorbent also has secondary pollution problem and exists.And for example adsorption system is when designing in the runner mode, because of being limited to the non-refractory characteristic of peripheral packing material between each adsorbent of runner, and whole runner must be disintegrated into the original unit bulk of adsorbent, row combination again after the roasting regeneration, inconvenience very.
The aging shortcoming that is difficult for regeneration in order to improve long-term use of existing adsorbent, the object of the present invention is to provide a kind of renovation process of waste gas adsorbing and treating system, it is with a solvent clean or method of extraction, adsorption capacity has been reduced and can't be in the mode of regenerating on the continuous lines with the adsorbent or the adsorption system regeneration of general steam, hot-air or inert gas regeneration, to prolong the useful life of adsorbent.
The renovation process of a kind of waste gas adsorbing and treating system of the present invention is characterized in that directly will being deposited on the method that adsorbent surface or intrapore higher boiling chemical substance or oligomer clean, wash away and regenerate with method continuous on the line with the solvent that mixes.
Its cleaning solvent is that wherein one or two or more kinds the solvent of water, alcohol and ketone forms; Wherein alcohol is meant that carbon number is one to four straight chain alcohol or branched-chain alcoho, and ketone is meant that carbon number is one to four straight chain, side chain or cyclic ketone or furans.
The ratio of its cleaning solvent is a water: alcohol is 1: 0 to 1: 99; Water: ketone is 1: 0 to 1: 99, and temperature is 20-80 ℃ a mixed solvent.
The mode of its cleaning is carried out for the mode of spraying continuously or soaking with nozzle.
Its adsorption system can be rotary-type, the pattern of fluidized bed formula or fixed bed.
The adsorbent of its use comprises zeolite, activated carbon, macromolecule resin and laminated soil.
Its runner adsorption system comprises: vertical type, horizontal or column type.
For further understanding effect of the present invention and feature, below in conjunction with drawings and Examples the present invention is made a detailed description, wherein:
Fig. 1 is the schematic diagram of spray-type regenerative system;
Fig. 2 is the schematic diagram of immersion type regenerative system.
The present invention promptly is to have high solvent mixed solvent, with nozzle with mixed solvent before desorption manipulation, adsorbent is sprayed cleaning, or cleaning solvent is loaded in the storage tank, the adsorbent of certain part in the adsorption system is soaked in wherein, and the intrapore height that makes adsorbent boil obstruction adsorption capacities such as organic substance, oligomer or dust substance dissolves or wash away, the inventive method can be adopted the operation of batch formula, also can adopt continued operation.Wherein the method for especially spraying is specially adapted to the adsorption system of continued operation, for example rotary-type absorption concentration systems, or fluidized bed adsorption system.In rotary-type absorption concentration systems, can add a cleaning area in addition at the front end in rotary wheel regeneration district.Install whole row's nozzle in cleaning area, cleaning solvent is sprayed on adsorbent in the runner, and boil organic matter or oligomer of its intrapore height washed away, Fig. 1 i.e. the schematic diagram of system and device for this reason.As take immersion way when operation, can establish a solvent feed tank in the Lower Half of runner, cleaning fluid is equipped with in inside, clean (as shown in Figure 2) when runner turns to Lower Half, with the high-boiling components matter or the oligomer dissolving that residue in the adsorbent duct, this can be with the adsorbent cyclic regeneration in the runner, for increasing the benefit of cleaning, can in groove, install the ultrasonic washer, but because the cleaning force of solvent of the present invention is enough, the effect of adding the ultrasonic concussion is not remarkable.As adsorption system is the fluidized bed formula, then can set up a hydro-peening district at the leading portion that enters regeneration desorption district, and the high-boiling components matter or the oligomer that are attached in the adsorbent are washed away.
Solvent used in the present invention mainly is that wherein one or two or more kinds the solvent with water, alcohol and ketone forms.It is one to four alcohols that alcohol can be selected the carbon containing number, for example methyl alcohol, ethanol, isopropyl alcohol and alcohol etc. down, and ketone then can be selected acetone, methyl ethyl ketone, oxolane ... etc.The usage ratio of solvent is a water: alcohol is between 1: 0 to 1: 99 (mol ratio); The ratio of water and ketone then is between 1: 0 to 1: 99 (mol ratio), and with water: alcohol was at 1: 0 to 1: 50, and water: ketone is best between 1: 0 to 1: 50.The apparatus of solvent is looked the kind of high boiling substance residual in the adsorbent or polymer and content, and different generally speaking every liter adsorbent is advisable with 0.01-10 litre solvent clean and different, wherein the best be every liter with between the 0.2-5 litre.Though too much solvent can improve the ability of adsorbent reactivation, there is no special benefit.Because this type of mixed solvent has high dissolving power for high boiling substance and oligomer, via the adsorbent after the inventive method regeneration, its adsorption capacity can return to more than 99% of original adsorption capacity, and adsorbent itself there is no any efflorescence or degradation loss, does not need to replenish separately adsorbent again.
Advantage of the present invention is to operate at low temperatures, can reach the ability that makes adsorbent reactivation.Use renovation process of the present invention to carry out that the regeneration of adsorbent is appropriate to the occasion to be carried out between room temperature-80 ℃, and with best between the room temperature-50 ℃, when operating more than 80 ℃, though can slightly shorten the time of cleaning, the loss of cleaning solvent easily caused, and must replenish.In addition, another advantage of the present invention is that cleaning solvent is reusable, and the solvent after the cleaning can be recycled after collecting filtering solid part, only need do a spot of replenishing and get final product.
Another characteristics of the present invention are can the intermittently operated of automation mode; when the exhaust emissions after adsorption system is handled conforms with in the scope of environmental regulations (import and export of adsorption system can be established the air continuous monitoring device); can be by general suction, desorption manipulation; need not cleaning operation; when monitoring system shows that the air concentration of emission continues to rise and during near the concentration of environmental regulation; the nozzle that cleans is opened automatically; carry out cleaning operation; do not need shutdown operation can make the purpose of whole adsorption system and adsorbent reactivation, not only save manpower and can guarantee the quality of exhaust.
Be the convenient superiority of the present invention of understanding, specify for example that below waste gas of the present invention absorption place buries the characteristic of system regeneration method, simultaneously also with other renovation process relatively.Bury effect everywhere and be the enchashment industry and use adsorption capacity to drop to not to be inconsistent adsorbent in the environmental protection exhaust rules prescribed limit at present, or with the result of mounting equipment to industry exhaust on-the-spot test.The industry exhaust gas discharged is with gas chromatograph chromatograph (GC), and gaseous mass chromatography instrument (GC-MASS) and full carbon-hydrogen analyzer (THC, FID) etc. carry out qualitative and be quantitative.Treatment effeciency in the embodiment calculates according to following formula.The all examples of following formula are only applicable to representative special case of the present invention, yet scope of the present invention is not limited to these embodiment:
Embodiment one
Certain industry waste gas composition includes methyl-sulfoxide 0-15PPM, monoethanolamine 20-30PPM, N-methyl-pyrrole noise made in coughing or vomiting ketone 1-10PPM, DMDS alcohol 0.5-10PPM, ethylene glycol 5-20PPM, isopropyl alcohol 20-200PPM, the waste gas air quantity is 55000 cubic metres/hour, delivery temperature is between 30-50 ℃, is to be that 3900mm thickness is that the zeolite runner adsorption system of 400mm is carried out the waste gas concentration with a diameter at present, adsorb saturated part then with 180 ℃ hot-air continuously with rotary wheel regeneration.Its concentration of concentrated gas that blows out through hot-air is about ten times (cycles of concentration is 10) of inlet gas concentration, through importing an oxidation Decomposition stove, resolves into carbon dioxide and water.The purifying exhaust air of runner inspissator discharging is formed by analysis as a result, and its initial stage treatment effeciency is 97% (with FID analyzing total hydrocarbons), treatment effeciency through continued operation runner after five months drops to 89% gradually, again with regenerated with hot air, also can't promote treatment effeciency, oxidation Decomposition heater exhaust result by analysis remains between the 99-100%, clean 3 hours (as Fig. 1＜b〉shown in) through spraying continuously with 40 ℃ hot water with method of the present invention, per hour water consumption is 1 ton, water after washing is reused about 1.1 tons of total water amount again after collection is filtered and replenished.The purifying exhaust air that adsorption treatment after the regeneration is discharged is formed result by analysis, and it is 95% that processing improves economic returns.
Embodiment two
Certain discharging waste gas includes isopropyl alcohol 30-500PPM; Acetone 20-100PPM; Dimethyl mercaptan 2-15PPM; Trimethyl silanol 4-15PPM; The about 10PPM of toluene; The about 20PPM of tetramethyl two silicon ammoniums; Air quantity is 25000 cubic metres/hour, and delivery temperature is 45 ℃, through being that 2500mm thickness is that the activated carbon runner of 350mm carries out concentration, its equipment for after-treatment such as embodiment one with a diameter.Adsorbing saturated activated carbon is that 130 ℃ nitrogen is regenerated with temperature.To handle benefit be 95% to the Purge gas of runner discharging its initial stage as a result by analysis, and after the place buried three months continuously, it was handled benefit and drops to 73%, in kind regenerated again, also can't promote treatment effeciency.Warp is with the method with embodiment one, only change cleaning solvent into water: methyl ethyl ketone=1: 45, and water: isopropyl acetone=1: 30, with room temperature continuous wash 3 hours, the total consumption of solvent is 1.6 tons, and it is 93% that the purifying exhaust air that absorption processing system discharged after the result regeneration forms by analysis that result treatment improves economic returns.
Embodiment three
Waste gas as embodiment one is formed, bury with built-in 20 liters spherical activated carbon miniature fluid bed adsorption system place, per hour handling air quantity is 1 cubic metre, adsorbing saturated activated carbon send and makes the renewing zone, regenerate with the nitrogen that is heated to be 150 ℃, activated carbon after the regeneration is sent back in the adsorbent bed with air and is adsorbed, and the solvent gas that desorption comes out reclaims after condensation.To bury efficient be 96% to purified waste gas initial stage place as a result by analysis, and after two months, the treatment of waste gas decrease in efficiency is 85% through continued operation, and through with water: butanols is 10: 40; Water: oxolane is that 50: 10 mixed solvent cleans; The activated carbon that regeneration is good enter the renewing zone with the remaining cleaning solvent of 150 ℃ nitrogen blow-off after, sending into adsorption zone carries out adsorption operations, the result of purifying exhaust gas by analysis, treatment effeciency returns to 95%, total cleaning solvent consumption is 100 liters.Embodiment four
Form as the waste gas that embodiment two is identical, carry out waste gas purification with the double-tower type ADSORPTION IN A FIXED BED system of the built-in 50 liters of strip activated carbon of every tower and handle.Wherein a tower is an adsorbed state, and another tower is that 120 ℃ steam carries out desorption and regeneration with temperature then, the gas that purifies the back discharging by analysis as a result the initial stage treatment effeciency be 92%, after two weeks of continued operation, treatment effeciency drops to 60%, continues also can't lifting place bury efficient with steam regeneration.Generate through observing activated carbon surface adularescent shot-like particle.Through with a water: oxolane is that 90: 10, temperature are that 50 ℃ mixed solvent soaked one day, after the cleaning solvent eliminating, again with after 100 ℃ the cleaning solvent blowing of nitrogen with remnants in the activated carbon, carry out the purification adsorption treatment of waste gas again, bury efficient and revert to 90% at the place as a result, activated carbon does not have powder phenomenon-tion, does not need any replenishing.Comparative example one
As embodiment four identical operations, only change the method for regeneration, adsorption capacity among the embodiment four has been dropped to a wherein tower activated carbon of 60% takes out, carry out regeneration test with small-sized rotation regeneration kiln, through heating to 700 ℃, and feed steam (every liter of activated carbon feeds 0.25 liter steam) and regenerate, activated carbon after the regeneration is through screening, insert in the adsorption tower again after removing broken granule, carry out waste gas purification again and handle after replenishing 10 liters of fresh activated carbon, the efficient of exhaust-gas treatment is gone up to 86% as a result.
By the result of embodiment one to four renovation process of the exhaust treatment system of the inventive method as can be known, can effectively regenerate and to recover the adsorbent of adsorption capacity with general desorption method, and directly operate on the line, reduce the puzzlement of adsorbent loading and unloading, the phenomenon of not having adsorbent efflorescence or deterioration again, the operation time limit of increase adsorbent.
Claims (5)
1. the renovation process of a waste gas adsorbing and treating system, it is characterized in that directly will being deposited on the method that adsorbent surface or intrapore higher boiling chemical substance or oligomer clean, wash away and regenerate with method continuous on the line with the solvent that mixes, its cleaning solvent is that wherein one or two or more kinds the solvent of water, alcohol and ketone forms; Wherein alcohol is meant that carbon number is one to four straight chain alcohol or branched-chain alcoho, and ketone is meant that carbon number is one to four straight chain, side chain or cyclic ketone or furans, and the mode of its cleaning is carried out for the mode of spraying continuously or soaking with nozzle.
2. the renovation process of a kind of waste gas adsorbing and treating system according to claim 1 is characterized in that, the ratio of its cleaning solvent is a water: alcohol is 1: 0 to 1: 99; Water: ketone is 1: 0 to 1: 99, and temperature is 20-80 ℃ a mixed solvent.
3. the renovation process of a kind of waste gas adsorbing and treating system according to claim 1 is characterized in that, its adsorption system can be rotary-type, the pattern of fluidized bed formula or fixed bed.
4. the renovation process of a kind of waste gas adsorbing and treating system according to claim 3 is characterized in that, the adsorbent of its use comprises zeolite, activated carbon, macromolecule resin and laminated soil.
5. the renovation process of a kind of waste gas adsorbing and treating system according to claim 3 is characterized in that, its runner adsorption system comprises: vertical type, horizontal or column type.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN99109003A CN1102418C (en) | 1999-06-11 | 1999-06-11 | Regeneration method of waste gas adsorbing and treating system |
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| Application Number | Priority Date | Filing Date | Title |
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| CN99109003A CN1102418C (en) | 1999-06-11 | 1999-06-11 | Regeneration method of waste gas adsorbing and treating system |
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| CN1277069A CN1277069A (en) | 2000-12-20 |
| CN1102418C true CN1102418C (en) | 2003-03-05 |
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| CN99109003A Expired - Lifetime CN1102418C (en) | 1999-06-11 | 1999-06-11 | Regeneration method of waste gas adsorbing and treating system |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101406790B (en) * | 2007-10-09 | 2011-09-14 | 华懋科技股份有限公司 | Rotary real-time early warning device of adsorption runner |
| CN101862547B (en) * | 2009-04-14 | 2011-12-21 | 杰智环境科技股份有限公司 | Rotary solvent recovery device and method |
| CN101920153A (en) * | 2009-06-12 | 2010-12-22 | 杰智环境科技股份有限公司 | Cleaning regenerating unit and method of honeycomb-shaped adsorber |
| CN101961649B (en) * | 2010-10-19 | 2012-08-22 | 同济大学 | Regeneration method of air sampling adsorbing agent |
| TW201311336A (en) * | 2011-09-09 | 2013-03-16 | Ind Tech Res Inst | Adsorption unit, adsorption device and method for regenerating thereof |
| TW201400172A (en) * | 2012-06-20 | 2014-01-01 | Desiccant Technology Corp | Absorptive turning wheel replacement method |
| CN108854434B (en) * | 2017-05-15 | 2021-06-04 | 中国石油化工股份有限公司 | Method and device for treating refinery VOCs waste gas |
| CN113332830A (en) * | 2021-06-01 | 2021-09-03 | 南通大学 | Special regeneration method for zeolite rotating wheel |
| CN116585848B (en) * | 2023-06-28 | 2024-02-27 | 广州华科环保工程有限公司 | Method for concentrated collection and resource regeneration after organic waste gas dispersion treatment in printing and dyeing industry |
| CN117563384B (en) * | 2024-01-17 | 2024-04-05 | 江苏三吉利化工股份有限公司 | Furanol organic waste gas efficient recovery process and equipment |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62282639A (en) * | 1986-05-31 | 1987-12-08 | Kyoritsu Yuki Co Ltd | Regenerator provided with collecting sleeve |
| JPS63156542A (en) * | 1986-12-19 | 1988-06-29 | Kuraray Chem Kk | Method for regenerating activated carbon |
| US4957721A (en) * | 1988-06-28 | 1990-09-18 | Lonsinger Jack J | Process for regeneration of activated carbon |
| US5405812A (en) * | 1990-08-17 | 1995-04-11 | Steag Aktiengesellschaft | Method and arrangement for purifying a carbon-containing adsorption medium |
| CN2241015Y (en) * | 1996-04-26 | 1996-11-27 | 卞直旭 | Vibration type continuous internal heated active carbon regenerating furnace |
-
1999
- 1999-06-11 CN CN99109003A patent/CN1102418C/en not_active Expired - Lifetime
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62282639A (en) * | 1986-05-31 | 1987-12-08 | Kyoritsu Yuki Co Ltd | Regenerator provided with collecting sleeve |
| JPS63156542A (en) * | 1986-12-19 | 1988-06-29 | Kuraray Chem Kk | Method for regenerating activated carbon |
| US4957721A (en) * | 1988-06-28 | 1990-09-18 | Lonsinger Jack J | Process for regeneration of activated carbon |
| US5405812A (en) * | 1990-08-17 | 1995-04-11 | Steag Aktiengesellschaft | Method and arrangement for purifying a carbon-containing adsorption medium |
| CN2241015Y (en) * | 1996-04-26 | 1996-11-27 | 卞直旭 | Vibration type continuous internal heated active carbon regenerating furnace |
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