CN103240059A - Preparation method of active carbon for oil gas recovery - Google Patents
Preparation method of active carbon for oil gas recovery Download PDFInfo
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- CN103240059A CN103240059A CN2013102080754A CN201310208075A CN103240059A CN 103240059 A CN103240059 A CN 103240059A CN 2013102080754 A CN2013102080754 A CN 2013102080754A CN 201310208075 A CN201310208075 A CN 201310208075A CN 103240059 A CN103240059 A CN 103240059A
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Abstract
The invention discloses a preparation method of active carbon for oil gas recovery, which comprises the following steps of: steeping the plant straw with a particle size of 10-100 meshes and phosphoric acid with mass concentration of 50-85% at a certain mass ratio for a certain time at 70-100 DEG C, and putting into a reaction tank; putting the product in a carbonization furnace; heating to an activation temperature at a heating rate of 5-10 DEG C per minute in a nitrogen atmosphere, and preserving heat for a certain period of time at the temperature; after the activation is over, stopping heating, and reducing the temperature of the carbonization furnace to the room temperature in the nitrogen atmosphere; taking out the product and repeatedly flushing with deionized water; performing suction filtration until the pH value of the filtrate is greater than 6; and then, putting the flushed active carbon into an oven, and performing normal-pressure and vacuum drying respectively for 10-15 hours at 100-120 DEG C to obtain active carbon especially suitable for oil gas recovery. The active carbon product prepared by the method disclosed by the invention has high pore volume proportion, moderate pore diameter distribution and large specific surface area, greatly reduces the attenuation of adsorption capacity, is very suitable for oil gas recovery, has the characteristics of small investment and low operation cost, and also can be applied to the field of adsorption recovery of other organic gases.
Description
Technical field:
The present invention relates to a kind of adsorbent that in the oil gas absorbing recovery device, uses, relate in particular to a kind of acticarbon that in the oil gas absorbing recovery device, uses
Technical background:
Oil product owing to have the restriction of technology and equipment now, will volatilize light hydrocarbon component, i.e. oil gas inevitably in exploitation, storage, processing, accumulating and sales process.Oil gas and air Mixture are not only brought environmental pollution and disaster hidden-trouble, also cause the loss of oil product quantity and quality to descend.Oil gas reclaims the market demand that very huge reality and potentiality is arranged.Oil gas reclaims can prevent the atmosphere pollution that oil gas volatilization causes, and eliminates safe hidden trouble, and by improving rate of energy, reduces economic loss, thereby obtains considerable benefit repayment.Fields such as exhaust gas discharged, recycling associated gas when the oil gas recovery technology can also be used for administering the production chemical product simultaneously.Oil gas reclaims common method at present absorption method, absorption process, condensation method and membrane separation process.The difficult point that oil gas reclaims absorption process is suitable absorbent, needs big, the easy absorbent of separation oil and gas method of exploitation absorption oil and gas content; Condensation method is to utilize Refrigeration Technique that the heat of oil gas is cemented out, realize the direct conversion of oil-gas component from the gas phase to the liquid phase, its technological principle is simple, handling safety, but want needs up to standard to drop to very low temperature, power consumption is big, and exhaust emissions concentration will reach the standard that is lower than 25mg/L, and investment and operating cost all will significantly increase.Membrane separation process utilizes special polymeric membrane hydro carbons to be had the characteristics of penetrated preferably, allow oil gas and air Mixture under the promotion of certain pressure, make oil gas molecule penetrated preferably polymeric membrane, constituent of air then is trapped discharging, the oil gas transmission of enrichment is sent oil tank back to or is liquefied with additive method, its advanced technology, technology are simple relatively, and concentration of emission is low, rate of recovery height, its shortcoming is that investment is big, expensive, and membrane lifetime is short; Absorption method can reach high processing efficient, and concentration of emission is low, can reach the discharge index that is lower than 10mg/l, but its difficult point be need initial passivation easily, the sorbing material of desorption efficient height, long service life.The China made activated carbon absorption affinity generally has only about 7%, and the life-span is not long, will change once in general about 2 years, and it is very high to change an active carbon cost.Active carbon is physical adsorption process to the adsorption process of oil gas, and has the double characteristic of micropore filling and capillary condensation.The architectural feature of absorption, desorption process and active carbon is closely related.The active carbon for preparing suitable specific surface, pore volume and pore-size distribution is the key factor of improving absorption and desorption performance.The adsorbent that oil gas reclaims usefulness should have higher pore volume, micropore specific surface and suitable pore-size distribution.Acticarbon has higher cost performance, and the charcoal absorption performance degradation that aperture＜2nm, pore size distribution are narrower is very fast, after the multiple adsorb its influence particularly evident, be not suitable for recycling.The pore-size distribution of acticarbon is more favourable with the raising of desorption performance to absorption when 2～6nm, can obviously reduce the decay of adsorbance, progressively tends towards stability then, is suitable for oil gas especially and reclaims.
Activated carbon product mesopore volume ratio of the present invention is greater than 60%, and specific area is big, is very suitable for absorption method oil gas and reclaims use, has small investment, the characteristics that running cost is low, and the field is reclaimed in the absorption that can also be applied to other organic gas.
Summary of the invention:
The purpose of this invention is to provide a kind of method for preparation of active carbon for the oil gas recovery, characteristics are that preparation speed is fast, less demanding to equipment, the pore-size distribution of the acticarbon of preparation is mainly at 2～6nm, can obviously improve absorption and desorption performance to oil gas, reduce the decay of adsorbance, be suitable for oil gas especially and reclaim the field.
Process for preparing active carbon for the oil gas recovery of the present invention is as follows:
With particle diameter be the phosphoric acid of 10～100 purpose straws and mass concentration 50～85% with certain mass ratio, putting into reactive tank after dipping a period of time under 70～100 ℃ of temperature, and placing in the retort.Under nitrogen atmosphere, be heated to activation temperature with the heating rate of 5～10 ℃/min, under this temperature, be incubated a period of time.Stop heating after activation finishes, the retort temperature is down to room temperature under nitrogen atmosphere.Product taken out washes repeatedly with deionized water, suction filtration, to pH value of filtrate greater than 6, the active carbon after will washing is then put into baking oven and was carried out normal pressure and vacuum drying respectively each 10～15 hours under 100～120 ℃, obtains being used in particular for the active carbon of oil gas recovery.
Advantage of the present invention:
Preparation method of the present invention is simple, and equipment requires low, small investment, and running cost is low.The acticarbon mesopore volume ratio height of preparation, pore-size distribution is moderate, the aperture mainly is distributed in 2～6nm, specific area is big, can obviously improve absorption and desorption performance to oil gas, reduce the decay of adsorbance greatly, be suitable for oil gas especially and reclaim the field, exhaust gas discharged field in the time of can also being used for administering the production chemical product.
The specific embodiment:
1. embodiment 1
The phosphoric acid that with particle diameter is 10～18 purpose wood fragments bits and 50% mass concentration in 100 ℃ temperature under flood 6h after is put into reactive tank and is placed retort with mass ratio at 1: 2.0.Heating rate with 10 ℃/min under nitrogen atmosphere is heated to 550 ℃ of activation temperatures, is incubated 1h under this temperature.Stop heating after activation finishes, continue logical nitrogen temperature to the stove and be down to room temperature, product is taken out wash repeatedly with deionized water, suction filtration is so that pH value of filtrate greater than 6, was carried out normal pressure and vacuum drying respectively each 15 hours with the active carbon after washing under 100 ℃.Obtain active carbon.The active carbon structural characteristic parameter sees Table 1.
2. embodiment 2
With particle diameter be the phosphoric acid of 18～35 order cocoanut shells and 60% mass concentration with mass ratio 1: 6.0 in putting into reactive tank and place retort behind the dipping 48h under 90 ℃ of temperature.Heating rate with 5 ℃/min under nitrogen atmosphere is heated to 400 ℃ of activation temperatures, is incubated 3h under this temperature.After finishing, activation stops heating, continue logical nitrogen temperature to the stove and be down to room temperature, product is taken out wash suction filtration with deionized water repeatedly, so that pH value of filtrate greater than 6, is put into baking oven with the active carbon after washing and was carried out normal pressure and vacuum drying respectively each 15 hours under 120 ℃.Obtain active carbon.The active carbon structural characteristic parameter sees Table 1.
3. embodiment 3
With particle diameter be the phosphoric acid of 35～60 purpose mao bamboons and 70% mass concentration with mass ratio 1: 4.5: in putting into reactive tank and place retort behind the dipping 12h under 80 ℃ of temperature.Heating rate with 10 ℃/min under nitrogen atmosphere is heated to 450 ℃ of activation temperatures, is incubated 2h under this temperature.After finishing, activation stops heating, continue logical nitrogen temperature to the stove and be down to room temperature, product is taken out wash suction filtration with deionized water repeatedly, so that pH value of filtrate greater than 6, is put into baking oven with the active carbon after washing and was carried out normal pressure and vacuum drying respectively each 10 hours under 100 ℃.Obtain active carbon.The active carbon structural characteristic parameter sees Table 1.
4. embodiment 4
Be 60～100 order corncobs with the phosphoric acid of 85% mass concentration with impregnating ratio 1: 4.0 in putting into reactive tank and place retort behind the dipping 24h under 70 ℃ of temperature with particle diameter.Heating rate with 10 ℃/min under nitrogen atmosphere is heated to 600 ℃ of activation temperatures, is incubated 1h under this temperature.After finishing, activation stops heating, continue logical nitrogen temperature to the stove and be down to room temperature, product is taken out wash suction filtration with deionized water repeatedly, so that pH value of filtrate greater than 6, is put into baking oven with the active carbon after washing and was carried out normal pressure and vacuum drying respectively each 10 hours under 120 ℃.Obtain active carbon.The active carbon structural characteristic parameter sees Table 1.
The BET specific area of table 1 active carbon, pore volume, pore-size distribution reach the adsorption desorption performance to the 93# gasoline vapour
Claims (5)
1. one kind is used for the method for preparation of active carbon that oil gas reclaims, and it is characterized in that process is as follows:
(1) with particle diameter be the phosphoric acid of 10～100 purpose straws and mass concentration 50～85% with certain mass ratio, under 70～100 ℃ of temperature, flood a period of time.
(2) above-mentioned material is put into reactive tank, and places in the retort.Under nitrogen atmosphere, be heated to activation temperature with the heating rate of 5～10 ℃/min, under this temperature, be incubated a period of time.Stop heating after activation finishes, the retort temperature is down to room temperature under nitrogen atmosphere.
(3) product taken out wash repeatedly with deionized water, suction filtration, to pH value of filtrate greater than 6, the active carbon after will washing then carried out normal pressure and vacuum drying respectively each 10～15 hours under 100～120 ℃, obtain being used in particular for the active carbon that oil gas reclaims.
2. method for preparation of active carbon according to claim 1 is characterized in that, the mass ratio of described straw and phosphoric acid is 1: 2～1: 6.
3. method for preparation of active carbon according to claim 1 is characterized in that, described dip time is 6～48 hours.
4. method for preparation of active carbon according to claim 1 is characterized in that, described activation temperature is 400～600 ℃.
5. method for preparation of active carbon according to claim 1 is characterized in that, described soak time is 1～3 hour.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103480336A (en) * | 2013-10-10 | 2014-01-01 | 东南大学 | Modified biomass activated coke mercury removal adsorbent and preparation method thereof |
| CN103521027A (en) * | 2013-09-25 | 2014-01-22 | 江苏中远环保科技有限公司 | Oxygen-removed oil gas recovery method and device |
| CN106315494A (en) * | 2016-08-28 | 2017-01-11 | 张哲� | Oil and gas recovery device for gasoline station |
| CN109107377A (en) * | 2017-06-22 | 2019-01-01 | 财团法人工业技术研究院 | Carbonized material, ozone removing apparatus, and method of removing ozone |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101648707A (en) * | 2009-08-27 | 2010-02-17 | 南京林业大学 | Preparation method of activated carbon with high pore volume |
| CN102398904A (en) * | 2011-10-20 | 2012-04-04 | 江西省七星炭材科技有限公司 | Preparation of fuel oil recovery special active carbon by taking mao bamboo leftovers as raw material and method thereof |
| US8377843B2 (en) * | 2005-12-16 | 2013-02-19 | Ut-Battelle, Llc | Activated carbon fibers and engineered forms from renewable resources |
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- 2013-05-30 CN CN2013102080754A patent/CN103240059A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8377843B2 (en) * | 2005-12-16 | 2013-02-19 | Ut-Battelle, Llc | Activated carbon fibers and engineered forms from renewable resources |
| CN101648707A (en) * | 2009-08-27 | 2010-02-17 | 南京林业大学 | Preparation method of activated carbon with high pore volume |
| CN102398904A (en) * | 2011-10-20 | 2012-04-04 | 江西省七星炭材科技有限公司 | Preparation of fuel oil recovery special active carbon by taking mao bamboo leftovers as raw material and method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103521027A (en) * | 2013-09-25 | 2014-01-22 | 江苏中远环保科技有限公司 | Oxygen-removed oil gas recovery method and device |
| CN103480336A (en) * | 2013-10-10 | 2014-01-01 | 东南大学 | Modified biomass activated coke mercury removal adsorbent and preparation method thereof |
| CN103480336B (en) * | 2013-10-10 | 2016-03-16 | 东南大学 | A kind of modified biomass activates burnt demercuration adsorbent and preparation method thereof |
| CN106315494A (en) * | 2016-08-28 | 2017-01-11 | 张哲� | Oil and gas recovery device for gasoline station |
| CN109107377A (en) * | 2017-06-22 | 2019-01-01 | 财团法人工业技术研究院 | Carbonized material, ozone removing apparatus, and method of removing ozone |
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Application publication date: 20130814 |