CN101342439B - Hydrocarbons recovery method - Google Patents
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- CN101342439B CN101342439B CN200710012087.4A CN200710012087A CN101342439B CN 101342439 B CN101342439 B CN 101342439B CN 200710012087 A CN200710012087 A CN 200710012087A CN 101342439 B CN101342439 B CN 101342439B
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Abstract
The present invention relates to a hydrocarbon recovery method, which adopts solid absorbent to adsorb hydrocarbon. Mixed gas containing hydrocarbon first passes through uninflammable inorganic absorbent and then inflammable absorbent; the uninflammable inorganic absorbent contains silica gel, zeolite or alumina; the inflammable absorbent contains activated carbon or activated carbon fibers; and the volume ratio between the uninflammable absorbent and the inflammable absorbent is between 20 : 80 and 80 : 20. The absorbents are regenerated by adopting a vacuum regeneration method or a steam regeneration method. The present invention provides a method and a device which are used for the purification and recovery of high-concentration hydrocarbon waste gases (VOCs, organic waste gases, oil gas). Compared with the prior art, the method has the advantages of low temperature rise of the absorbents, high safety performance, high recovery benefit, etc., and the concentration of VOCs at the emission outlet of the device can meet the national emission standard. The method can be used in places and cases producing high-concentration waste hydrocarbon gases, such as oil tanks, oily sewage tanks, hydrocarbon produced in the process of oil filling in tankers and VOCs produced in the process of hydrocarbon processing.
Description
Technical field
The invention provides a kind of hydrocarbons recovery method, particularly adopt absorption method to reclaim the method for hydro carbons.
Background technology
Crude oil, gasoline, some Chemical Solvents as organic solvents such as benzene,toluene,xylene workshop, coating in, contain or there is the light hydrocarbon component that volatility is very large, crude oil is in the processes such as the transportation of exploitation, transportation, storage, transfer, processing and converted products (gasoline, diesel oil etc.), transfer, sale, there is a large amount of oil vapour (oil gas) to spill in atmosphere, here the oil vapour of mentioning is commonly referred to VOCs, also referred to as non-methane hydrocarbon, the general designation hydrocarbon gas.
At oil refining enterprise, various storage tanks, sewage farm oil removal floation tank etc. also give out the hydro carbons of higher concentration, and these hydrocarbon component complexity, not only cause hydrocarbon loss, and often cause the odor pollution of surrounding enviroment.
Process the normally used method of this waste gas absorption method, burning method, Production by Catalytic Combustion Process, condensation method, absorption process etc. are arranged.In above-mentioned method, burning method, Production by Catalytic Combustion Process are ripe method, but these two kinds of methods all become CO by hydrocarbon fuel
2, hydro carbons can not be reclaimed, this is for resource growing tension today, the wasting of resources beyond doubt.Condensation method is the effective ways that reclaim hydro carbons, but will reach concerned countries standard (120mg/m
3) need-95 ℃ even lower, the operating cost costliness.And the absorption process purification efficiency is limited, waste gas outlet concentration is generally far away higher than emission request.Absorption method can make waste gas outlet concentration meet the requirement of environmental protection, this requirement of environmental regulation for increasingly stringent, and apparent and its application of the advantage of the method will continue.
Existing absorption method adopts the single hop bed to purification and the recovery of hydro carbons, usually adopt active carbon or NACF, patent CN03254728.5CN03254729.3, CN200410023944.7, CN02805902.6 and CN00118594.2 have all proposed by active carbon, hydro carbons to be adsorbed, and then carry out the method that steam desorb condensation recovery or vacuum desorption solvent absorption reclaim.Patent CN03254728.5CN03254729.3 has proposed respectively the device that a kind of absorption method oil gas reclaims, and adopts active carbon as adsorbent, and the hydro carbons after vacuum desorption absorbs as liquefied gas or diesel oil.Take active carbon or NACF as adsorbent, and its advantage is that adsorbance is larger, and adsorption efficiency is higher, and emission easily reaches the environmental protection index requirement.But, when its deficiency is in running to be difficult to control the higher oil gas of absorption temperature rise, particularly adsorption concentration, the active carbon bed temperature is very high, and obvious potential safety hazard is arranged.
Patent CN200410023944.7 has narrated a kind of device for recovering oil and gas, and import is equipped with flowmeter, and outlet is equipped with densimeter, is single tower.Although this patent import has the tonifying Qi safety measure, but still hot-spot in inevitable bed, cause the charcoal spontaneous combustion and cause danger.
A kind of method that patent CN02805902.6 proposes the steam desorb of charcoal absorption waste gas and reclaims.During this patent hydro carbons waste gas purification higher for concentration, there is equally the dangerous safety problem of the above-mentioned too high initiation of heat of adsorption.
Although the non-flammable adsorbent of other type also can be for the adsorption process of VOCs, in general adsorption efficiency is low, and the quantity of sorbent needed is larger, equipment investment increases, adsorbance when VOCs penetrates is lower, and the processing of need regenerating frequently, make troubles to operation.
Summary of the invention
For the deficiencies in the prior art, the invention provides the hydrocarbons recovery method that a kind of security is good, the rate of recovery is high, the adsorbent life-span is long, can purify the occasion reclaimed for various hydrocarbon gas, occasion as oil gas volatilization, various oil storage tanks, oil depot stevedoring place, gas station etc. locate, the device of the high concentration hydro carbons distributed in petrochemical enterprise etc.
In hydrocarbons recovery method of the present invention, adopt the method for solid absorbent absorption, the hydrocarbon-containifirst gaseous mixture is first by the non-combustible inorganic adsorbent, then by flammable adsorbent, the non-combustible adsorbent comprises silica gel, molecular sieve or aluminium oxide etc., and flammable adsorbent comprises active carbon or NACF etc.The non-combustible adsorbent is 20: 80～80: 20 with flammable adsorbent volume ratio, preferably 40: 60～70: 30.The cumulative volume air speed of the gaseous mixture of hydrocarbon-containifirst during by solid absorbent is 200～5000h
-1.After adsorbent absorption is saturated, employing vacuum regeneration mode or the regeneration of steam regeneration, adopt at least two adsorbent equipment handover operations.
Through research, find, the incombustibility adsorbent of inanimate matter is in the hydro carbons adsorption process, and adsorption efficiency is lower, and hydrocarbons is easy to penetrate adsorbent bed, and the adsorption capacity that hydro carbons penetrates when adsorbent bed is lower.But, when if hydro carbons concentration is higher, its total adsorbance is not starkly lower than the adsorbent of other type.In addition, during the incombustibility adsorbent adsorbs hydrocarbons of inanimate matter, its exotherm is starkly lower than acticarbon.The present invention is in conjunction with the characteristics of the dissimilar adsorbent of two classes, gaseous mixture contact by the first hydrocarbon-containifirst of inanimate matter incombustibility adsorbent, now the hydrocarbon concentration in gaseous mixture is higher, be conducive to improve the adsorbance of inanimate matter adsorbent, a large amount of hydro carbons is adsorbed in the low inanimate matter adsorbent of heat release simultaneously, and the temperature rise of adsorbent and air-flow is less.Because the adsorption efficiency of inanimate matter adsorbent is low, hydro carbons is easy to penetrate adsorbent bed, but now the concentration of hydro carbons reduces greatly, when follow-up active carbon class adsorbent contacts, the high characteristics of adsorption efficiency of acticarbon have been given full play to, before the adsorbent adsorbance reaches high value, emission, always in lower numerical value, can maintain longer service cycle.And now, the hydro carbons concentration in gaseous mixture reduces greatly, so the exotherm phenomenon on acticarbon obviously is eased, effectively avoided the too high and potential safety hazard that exists of flammable adsorbent temperature.
The accompanying drawing explanation
Fig. 1 is the inventive method absorption-vacuum desorption hydro carbons recovery process schematic flow sheet.
Fig. 2 is the inventive method absorption-steam desorption technique schematic flow sheet.
The specific embodiment
In hydrocarbons recovery method of the present invention, two kinds of dissimilar adsorbents can be seated in an adsorption tower in layering, also can load in series in two or more adsorption towers.During operation, at first the high concentration hydro carbons enters non-combustible adsorbent bed, non-combustible adsorbent is by after the absorption of high concentration hydro carbons, hydro carbons concentration in waste gas reduces greatly, enter the active carbon bed adsorption cleaning, at this moment because hydro carbons concentration in waste gas is lower, charcoal absorption heat is lower, has avoided spontaneous combustion or the explosion danger in the use procedure.Gas up to standard after purification is directly emptying.When the purified gas gas concentration exceeds standard, adsorption tower is switched, the processing of regenerating of saturated adsorption tower.
In running, reach relevant national standard as long as control the gas concentration of adsorption tower outlet, as Beijing " storage tank farm exhaust of oil control and limit value " (DB11/206-2003) in regulation, the purification efficiency of oil-gas recovery processing device (hereinafter to be referred as treating apparatus) should be lower than 98%; The concentration of emission for the treatment of apparatus should not be greater than 25g/m under standard state
3.When exit concentration surpasses the national regulation restriction, air-flow is switched to fresh adsorption tower and is adsorbed, and saturated adsorption tower carries out vacuum desorption or steam regeneration under the effect of vavuum pump, and the concentrated oil gas after desorb turns back to condenser system or absorption system is reclaimed.Certainly, the inventive method can realize that emission hydro carbons concentration is more lower than discharge standard.
In the present invention, inventive point is adsorption bed segmentation filling, and lower floor is non-combustible adsorbent, and upper strata is active carbon or NACF.Non-combustible adsorbent in the present invention is silica gel or modified silica-gel cheap and easy to get preferably, the upper strata adsorbent honest and clean active carbon be easy to get that preferably is situated between.Active carbon comprises plant material charcoal, ature of coal charcoal, malthenes charcoal, bone black, blood charcoal etc., preferably ature of coal charcoal and malthenes charcoal, most preferably ature of coal charcoal.Adsorbent can be selected the commodity adsorbent, also can be prepared by the existing knowledge in this area.Two class adsorbents all can be used the product of a tool granularity.Concrete shape comprises powdery, indefinite form particle, spherical, fibrous, textile-like etc., average grain diameter 1～10mm, preferably 2～6mm, most preferably 3～5mm.The specific area scope of adsorbent is at 200～3000m
2/ g, preferably 400～3000m
2/ g, consider most preferably 500～1500m of cost performance
2/ g average pore size 0.3～15nm, preferably 0.5～8nm, most preferably 1.0～3.0nm.Pore volume 0.2～2.0cm
3/ g, preferably 0.3～1.5cm
3/ g, most preferably 0.4～0.8cm
3/ g.
The adsorption method related in the present invention can be fixed bed, thermopnore and revolving bed, and preferred embodiment and operation be simple fixed bed all.The quantity of adsorption tower is 1～10, preferably 2～6, and optimum 2～4.
The recovery method related in the present invention is vacuum desorption-liquid absorption method, vacuum desorption-condensation method, steam blowing desorb-condensation method etc.Concrete grammar can be determined by this area general knowledge by the technical staff.
While adopting the vacuum desorption method, during desorb, can use the desorb purgative gas, also can not use, 0～2 times that the amount of desorb purgative gas is quantity of sorbent gets final product, preferably 0.5～1.5 times.But the desorb purgative gas can heat also normal temperature, temperature range environment temperature～200 ℃, preferred ambient temperature～150 ℃, most preferably environment temperature～70 ℃.Vacuum (absolute pressure value) scope during desorb in tower is 1KPa～20KPa, preferably 3～12KPa.
After vacuum desorption, while adopting liquid absorption to reclaim hydro carbons, absorbent can be high boiling point solvent oil and the special absorptive agent of gasoline, diesel oil and other stable chemical nature, as distillate or the artificial oil of boiling range between 180～450 ℃, initial boiling point is preferably higher than 220 ℃, 95% distillate is lower than 420 ℃, and solvent naphtha adds antioxidant, detersive to improve the stability of absorbent, is conducive to long-term use.Require 40 ℃ of kinematic viscosity of absorbent to be less than 20mm simultaneously
2/ s, preferably be less than 10mm
2/ s, condensation point requires lower than-5 ℃, preferably-10～-50 ℃.The selection of absorbent determine according to the concrete residing environment of hydrocarbon gas, if the hydrocarbon gas that large oil tank distributes, preferably gasoline or diesel oil absorbent, otherwise preferred high boiling point solvent oil or special absorptive agent.
While adopting condensation method to reclaim hydro carbons after vacuum desorption, condensation temperature scope-30 ℃～40 ℃, preferably 20 ℃～30 ℃ condensations.While moving in the time, under certain chilling temperature, when hydro carbons concentration is greater than the saturated vapor pressure at this temperature, hydro carbons is just understood condensation and is reclaimed, and the hydro carbons of all the other gaseous states turns back to adsorption tower and continues concentrated.
While adopting the steam desorb, the preferred hydrophobic adsorbent of non-combustible adsorbent, as dewatering silica gel, modified zeolite etc.Steam can be saturated vapor and also can be superheated steam, preferably superheated steam.Temperature range is 100 ℃～200 ℃, preferably 110～160 ℃.Quantity of steam is 2～8 times of adsorbent, preferably 3～5 times.
In the present invention, hydro carbons reclaims and adopts vacuum desorption, the method for liquid absorption, and technological process and device, as Fig. 1, also can adopt the steam desorb, and then the method for condensation reclaims hydro carbons, and flow process and device are shown in Fig. 2.
In Fig. 1 technological process, hydro carbons waste gas, under the draft of blower fan, enters adsorption tower A2 from lower to upper, at first, by non-combustible adsorbent bed 3, then after absorption, enters active carbon or bed of activated carbon fiber 4, finally by crossing the blower fan discharge.When active carbon or bed of activated carbon fiber penetrate (with country, relevant standard is as the criterion), the switching related valve, make hydro carbons waste gas carry out adsorption cleaning through non-combustible adsorbent bed 9 and active carbon or the bed of activated carbon fiber 10 of adsorption tower B8.Simultaneously, adsorption tower A2 carries out regenerative operation.Regeneration adopts vacuum regeneration, under vavuum pump 15 effects, passes into a small amount of purge gas, controls suitable vacuum, and adsorbent hydro carbons in adsorption tower A2 is desorbed, and purge gas can be temperature required through being heated to, and makes the hydro carbons desorb more thorough.The hydro carbons of separating sucking-off is concentrated gas, enters absorption tower 12, with suitable absorbent, absorbs processing, and unabsorbed a small amount of hydrocarbon gas returns to the adsorption tower entrance, with the hydrocarbon gas installed, together enters adsorption tower absorption.
In Fig. 2 technological process, hydro carbons waste gas, under the draft of blower fan, enters adsorption tower A2 from lower to upper, at first, by non-combustible adsorbent bed 3, then after absorption, enters active carbon or bed of activated carbon fiber 4, finally discharge.When active carbon or bed of activated carbon fiber penetrate (with country, relevant standard is as the criterion), the switching related valve, make hydro carbons waste gas carry out adsorption cleaning through non-combustible adsorbent bed 9 and active carbon or the bed of activated carbon fiber 10 of adsorption tower B8.Simultaneously, adsorption tower A2 carries out regenerative operation, and regeneration adopts the steam regeneration.Steam passes into the saturated adsorption tower of absorption and carries out desorb, and after desorb, high-temperature steam and hydrocarbon vapours together enter condenser 15, after condensation of gas, steam becomes condensed water, and hydrocarbon gas is condensed into liquid hydrocarbon, in the interior layering of oil water separator 16, condensed water elimination, liquid hydrocarbon reclaims.The part hydrocarbon gas be not condensed returns to the adsorption tower entrance, then enters the adsorption tower Adsorption Concentration, absorption-desorption-absorption successively.
Effect of the present invention: by the present invention, extended adsorbent service life, increased security, eliminated excessive active carbon spontaneous combustion and the explosion hazard that causes the too high generation of temperature rise of charcoal absorption heat.With pure absorption process, condensation method, compare, exhaust purification efficiency is high, invests low.With pure active carbon or carbon fiber adsorption and catalytic combustion method relatively, improve adsorbent service life, increase security.
Further illustrate implementation process and the effect of the inventive method below by embodiment, but limiting protecting scope not, those skilled in the art can determine according to the factors such as hydrocarbon content of processing gas the hydro carbons recycling condition of other similar gas.
Embodiment 1
The present embodiment adopts two sections absorption methods to process exhalation of tank gas, adopts gas mode of operation from the bottom to top, and total hydrocarbon concentration is 35% (volume), adopts vacuum desorption gasoline absorption process to reclaim hydro carbons, and lower floor's adsorbent is commercially available silica gel, specific area 713m
2/ g, pore volume 0.39ml/g, average pore size 2.2nm.Upper strata is commercially available active carbon, specific area 1077m
2/ g, pore volume 0.52ml/g, average pore size 1.5nm, absorption liquid is gasoline.The volume ratio of silica gel absorber and acticarbon is 60: 40, and the cumulative volume air speed is 1000h
-1, absorption 2h needs regeneration.After this PROCESS FOR TREATMENT, the exit gas total hydrocarbon concentration is less than 20ppm, the rate of recovery 100% (quality).22 ℃ of absorption environment temperatures, during absorption, the silica gel absorption bed temperature is the highest 40 ℃, the active carbon bed temperature 50 C.
Comparative example 1
This comparative example adopts process and the condition identical with embodiment 1, only has single a kind of acticarbon of employing.After processing, the exit gas total hydrocarbon concentration is less than 20ppm, the rate of recovery 100%, and absorption 2h needs regeneration.22 ℃ of absorption environment temperatures, during absorption, charcoal absorption bed temperature is the highest surpasses 80 ℃.Because the adsorption tower diameter of testing is only 40mm, when large-scale application,, there is certain self-ignition fatalness in the very possible hot-spot of active carbon bed temperature.In addition, in embodiment 1 and comparative example 1, regeneration frequency is basic identical, embodiment 1 is described and because use silica gel absorber, does not reduce whole adsorption capacity, if and only use silica gel absorber, adsorb 1～1.5h discharge gas and surpass environmental protection standard, need regeneration.
Embodiment 2
In the present embodiment, waste gas is 1% (volume) toluene, and lower floor is commercially available zeolite, specific area 750m
2/ g, pore volume 0.4ml/g, upper strata is active carbon, specific area 884m
2/ g, pore volume 0.4ml/g, average pore size 1.5nm, the steam desorb, 25 ℃ of condensation temperatures, zeolite is 30: 70 with active carbon volume ratio, the cumulative volume air speed is 3000h
-1.Through after this PROCESS FOR TREATMENT, the outlet toluene concentration is less than 3ppm, the rate of recovery>99.99% (quality).28 ℃ of absorption environment temperatures, lower floor's adsorption temp is 35 ℃, active carbon level temperature is 45 ℃.
Embodiment 3
Press the process of embodiment 1, the volume ratio of silica gel absorber and acticarbon is 80: 20, and the cumulative volume air speed is 800h
-1, adsorb and within 2 hours, need regeneration.After this PROCESS FOR TREATMENT, the exit gas total hydrocarbon concentration is less than 20ppm, the rate of recovery 100% (quality).22 ℃ of absorption environment temperatures, during absorption, the silica gel absorption bed temperature is the highest 40 ℃, the active carbon bed temperature 50 C.
Claims (6)
1. a hydrocarbons recovery method, adopt the method for solid absorbent absorption, the hydrocarbon-containifirst gaseous mixture is first by the non-combustible inorganic adsorbent, then by flammable adsorbent, the non-combustible inorganic adsorbent comprises silica gel, molecular sieve or aluminium oxide, and flammable adsorbent comprises active carbon or NACF; The non-combustible adsorbent is 20: 80～80: 20 with flammable adsorbent volume ratio.
2. the cumulative volume air speed of the gaseous mixture that in accordance with the method for claim 1, it is characterized in that described hydrocarbon-containifirst during by solid absorbent is 200～5000h
-1.
3. in accordance with the method for claim 1, it is characterized in that employing vacuum regeneration mode or the regeneration of steam regeneration after adsorbent absorption is saturated.
4. in accordance with the method for claim 1, it is characterized in that adsorption process adopts at least two adsorbent equipment handover operations.
5. in accordance with the method for claim 1, it is characterized in that non-combustible adsorbent and flammable adsorbent volume ratio are 40: 60～70: 30.
6. in accordance with the method for claim 1, it is characterized in that described non-combustible inorganic adsorbent and flammable adsorbent layering are seated in an adsorption tower, or load in series is in two or more adsorption towers.
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| CN101898071B (en) * | 2009-05-25 | 2012-09-12 | 中国石油化工股份有限公司 | Method for treating sulfur- and hydrocarbon-containing foul waste gas |
| CN102125792A (en) * | 2010-01-14 | 2011-07-20 | 哈尔滨天源石化工程有限责任公司 | New process for recovering oil gas by dual-layer bed formed by two adsorbents |
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| 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 |
| CN109603420A (en) * | 2018-11-06 | 2019-04-12 | 杨皓 | A kind of activation method of decarburization pressure-swing absorber silica gel |
| CN109513311B (en) * | 2019-01-16 | 2022-03-04 | 上海环境保护有限公司 | Waste gas treatment method for realizing high-efficiency energy-saving dynamic fluidized bed graded adsorption |
| CN110252080A (en) * | 2019-07-05 | 2019-09-20 | 昆山澳纳森节能环保科技有限公司 | VOC organic waste gas treatment device |
| CN110479028A (en) * | 2019-08-28 | 2019-11-22 | 中天科技精密材料有限公司 | A kind of oil vapor treatment system |
| CN111471478A (en) * | 2020-04-14 | 2020-07-31 | 青岛飞普思环保科技有限公司 | Method for reducing hot spot temperature of adsorption bed in oil gas recovery process by adsorption method |
| CN113599967A (en) * | 2021-08-13 | 2021-11-05 | 江苏锦东环境科技有限公司 | VOCs gaseous emission handles and uses adsorption tower |
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