CN103623774A - Method for preparing modified activated carbon used for fuel oil desulphurization - Google Patents
Method for preparing modified activated carbon used for fuel oil desulphurization Download PDFInfo
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Abstract
The invention discloses a method for preparing modified activated carbon used for fuel oil desulphurization. The method comprises following steps: adding distilled water to a reactor, adding sodium hydroxide solution to adjust the PH in a range of 6.8-14.3, adding activated carbon, adding mixed gas composed of ozone and air while stirring, carrying out an oxidation reaction on the surface of the activated carbon, taking out the activated carbon after the reaction is completed, flushing the activated carbon by distilled water and drying the activated carbon, and cooling the activated carbon to room temperature, so that the modified activated carbon is obtained, and the modified activated carbon can be used for adsorbing organic thiophene sulfide in the fuel oil. The activated carbon is modified in a liquid phase via the ozone, so that acidic oxygen-containing groups on the surface of the activated carbon are remarkably increased, adsorption capacity for the organic thiophene sulfide in the fuel oil is remarkably increased, and the mass of the modified activated carbon is not decreased.
Description
Technical field
The invention belongs to sorbing material field, relate to the preparation of oil product medium sulphide content sorbing material, be specifically related to a kind ofly utilize the modification of ozone liquid phase for the preparation of the method for the modified activated carbon of fuel desulfuration.
Background technology
Along with human society modernization degree is accelerated, the use amount of various motorized vehicles and vessels is rapid growth also.A large amount of automobiles that use can be to a large amount of discharges of environment containing SO
2waste gas.The SO of discharge
2not only human respiratory tract and lung are produced to injury, carcinogenic, also the generation of NOx and particle is had to obvious facilitation, meanwhile can form acid rain again, corrosion building and industrial equipment, destroy outdoor historical relic, cause forest and crops death etc., heavy damage ecological environment.For Global Sustainable Development, every country is formulated the sulfur content in strict regulation limitations fuel oil in succession.Therefore, produce ultra-clean fuel oil and " zero sulphur " fuel oil and become the technological challenge that global oil refining enterprise and petrochemical industry face.
Technology for fuel desulfuration can be divided into two large classes at present: (1) hydrodesulfurization technology; (2) non-hydrodesulfurization, comprises adsorption deeply desulfurization, alkylating desulfurization, abstraction desulfurization, oxidation sweetening and biological desulphurization etc.Traditional hydrodesulfurization technology can remove most of sulfide in fuel oil, weak point is under HTHP, to carry out, not only consuming a large amount of hydrogen but also octane number significantly loses, in addition, for thiophene-type sulfide, especially to many rings organic sulfur, because its space steric effect makes to be difficult to it is carried out to deep removal.
Adsorption deeply desulfurization belongs to a kind of of non-hydrodesulfurization, because it is simple to operate, can carry out deep desulfuration to fuel oil under normal temperature, normal pressure, can obtain ultra-clean fuel oil and " zero sulphur " fuel oil thereby be subject to extensive concern.
Active carbon is cheap, aboundresources not only, and there is huge specific area, prosperity to pore structure and abundant surface chemistry group, it has compared with width pore-size distribution, can overcome again the sterically hindered obstacle of partial vulcanization thing, can adsorb various organic sulfur compounds in fuel oil.[the Anning Zhou such as SONG, Xiaoliang Ma, and Chunshan Song, Liquid-Phase Adsorption of Multi-Ring Thiophenic Sulfur Compounds on Carbon Materials with Different Surface Properties, J. Phys. Chem. B 2006,110,4699-4707] the serial active carbon of preparing with different raw material is carried out to Study on adsorption properties to the organic sulfur in fuel oil, find that active carbon can effectively adsorb the various organic sulfurs in fuel oil.Although it has huge specific area active carbon, its adsorption capacity to part thiophene phenol sulfides such as benzo thiophene phenol BT in fuel oil is still not high enough.
To organic thiophenic sulfur compound, the adsorbance on active carbon has material impact to Surface Groups of Active Carbons, and acidic-group is more, and its adsorption capacity to organic thiophenic sulfur is larger.Therefore by oxidizing process, to activated carbon modified, can improve its total surface acidic-group concentration, increase the adsorption capacity to organic thiophenic sulfur.As [R.N.Fallah such as R.N.Fallah, S.Azizian, Removal of thiophenic compounds from liquid fuel by different modified activated carbon cloths, Fuel Processing Technology, 2012, 93, 45 – 52] apply respectively nitric acid, sulfuric acid and hydrochloric acid solution carry out surface oxidation treatment to active carbon cloth, effectively improved the acidic-group concentration of active carbon cloth material surface, active carbon cloth after modification is obviously increased the adsorption capacity of organic thiophenic sulfur, yet the weak point of this acid treatment method has been residual many acid waste liquids, contaminated environment, need further to process.In addition, [the Moxin Yu such as Yu Moxin, Zhong Li. Effect of thermal oxidation of activated carbon surface on its adsorption towards dibenzothiophene. Chemical Engineering Journal, 2009, 148, 2-3, 242-247] application of air thermal oxidation method modified activated carbon improved the acid oxy radical of activated carbon surface, significantly improved its absorption to dibenzothiophenes, but use this method of modifying to cause quality of activated carbon loss serious, and the temperature of air thermal oxide is higher, charcoal mass loss is more serious.
Summary of the invention
The object of the invention is to for active carbon itself not high enough to the adsorbance of benzothiophene, traditional air thermal oxidation method carries out the shortcoming that surface modification can cause quality of activated carbon severe attrition, provide a kind of use ozone in liquid phase modification for the preparation of the method for the modified activated carbon of fuel desulfuration.Method of the present invention keeps again the quality of active carbon itself not suffer a loss when effectively increasing the acid oxy radical of activated carbon surface, and the modified activated carbon of preparing has high absorption property to organic thiophenic sulfur compound.
With traditional air thermal oxidation method modified activated carbon, when temperature is during higher than 220 ℃, a part for active carbon is oxidized by transition and burns, and the mass loss of carbon is serious; If process active carbon in gas phase with ozone, because ozone is very strong oxidant, even at room temperature, active carbon also can burn rapidly.And the present invention is placed in the aqueous solution active carbon, ozone is passed in the aqueous solution and activated carbon surface generation oxidation reaction, because the intensity of oxidation reaction has been controlled in the existence of water effectively, active carbon can not burn, thereby can reach when having increased activated carbon surface acidic-group, avoid again quality of activated carbon to be subject to loss.
In order to achieve the above object, the present invention has adopted following technical scheme.
A preparation method for the modified activated carbon of fuel desulfuration, comprises the following steps:
(1) in reactor, add distilled water, adding sodium hydroxide solution to regulate pH value is 6.8 ~ 14.3, then adds active carbon, passes into while stirring the mist of ozone and air, and active carbon is carried out to surface oxidation reaction;
(2) after above-mentioned reaction finishes, active carbon is taken out, use distilled water flushing post-drying, be cooled to room temperature, make the modified activated carbon for fuel desulfuration.
In step (1), the molar concentration of described sodium hydroxide solution is 1 ~ 5mol/L; The temperature of described distilled water and sodium hydroxide solution is 15 ~ 35 ℃; The mass volume ratio of described active carbon and distilled water is 1:(10 ~ 30) g/mL.
In step (1), in described mist, the mass body volume concentrations of ozone is 15 ~ 65mg/L; The flow of described mist is 60 ~ 120mL/min.
The present invention also provides described modified activated carbon for adsorbing organic thiophenic sulfur of fuel oil.
Compared with prior art, tool has the following advantages in the present invention:
(1) the present invention is placed in the aqueous solution active carbon, ozone is passed in the aqueous solution and activated carbon surface generation oxidation reaction, because the intensity of oxidation reaction has been controlled in the existence of water effectively, active carbon can not burn, thereby can reach, increased activated carbon surface acidic-group, improve the adsorption capacity of active carbon to thiophenic sulfur compound in fuel oil, avoided again quality of activated carbon to be subject to loss;
(2) compare with traditional thermal oxidation method, the present invention has advantages of that quality of activated carbon is not subject to loss; Compare with traditional impregnating metal salt method, active carbon prepared by the present invention has higher adsorption capacity to thiophenic sulfur compound;
(3) raw materials of the present invention is with low cost, and raw material is easy to get;
(4) easy to operate, the safety of the present invention, environmentally safe.
accompanying drawing explanation:
When Fig. 1 is 30 ℃, modified activated carbon and the adsorption isotherm of original activity charcoal to organic thiophenic sulfur of embodiment 1 ~ 3 preparation.
When Fig. 2 is 30 ℃, modified activated carbon and the adsorption isotherm of original activity charcoal to organic thiophenic sulfur of embodiment 4 ~ 6 preparations.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described, but the scope of protection of present invention is not limited to this.
In embodiment, activated carbon granule used is of a size of 40 ~ 60 orders, and specific area is 2880.1m
2/ g.
embodiment 1
(1) Activated Carbon Pretreatment: active carbon washs to remove the inorganic and organic impurities of activated carbon surface successively through 0.1mol/L hydrochloric acid, 0.1mol/L NaOH and deionized water, at 110 ℃, dry standby after 2 hours;
(2) in the container of 100mL, add 35 ℃ of distilled water of 15mL, by the NaOH solution adjusting pH value of 35 ℃ of 1mol/L, be 6.8, then add the pretreated active carbon of 1g, at ambient temperature, ozone-the air gas mixture that is 32.5mg/L by ozone concentration while stirring blasts from container bottom equably, mixed gas flow is 80mL/min, and active carbon is carried out to surface oxidation reaction 0.5h;
(3) after reaction finishes, active carbon is taken out, use distilled water flushing post-drying, be cooled to room temperature, make the modified activated carbon for fuel desulfuration.
(1) Activated Carbon Pretreatment: active carbon washs to remove the inorganic and organic impurities of activated carbon surface successively through 0.1mol/L hydrochloric acid, 0.1mol/L NaOH and deionized water, at 110 ℃, dry standby after 2 hours;
(2) in the container of 100mL, add 10mL20 ℃ of distilled water, by the NaOH solution adjusting pH value of 20 ℃ of 1.5mol/L, be 10.3, then add the pretreated active carbon of 1g, at ambient temperature, ozone-the air gas mixture that is 32.5mg/L by ozone concentration while stirring blasts from container bottom equably, mixed gas flow is 80mL/min, and active carbon is carried out to surface oxidation reaction 1h;
(3) after reaction finishes, active carbon is taken out, use distilled water flushing post-drying, be cooled to room temperature, make the modified activated carbon for fuel desulfuration.
embodiment 3
(1) Activated Carbon Pretreatment: active carbon washs to remove the inorganic and organic impurities of activated carbon surface successively through 0.1mol/L hydrochloric acid, 0.1mol/L NaOH and deionized water, at 110 ℃, dry standby after 2 hours;
(2) in the container of 100mL, add 25mL15 ℃ of distilled water, then by the NaOH solution adjusting pH value of 15 ℃ of 5mol/L, be 14.3, then add the pretreated active carbon of 1g, at ambient temperature, ozone-the air gas mixture that is 32.5mg/L by ozone concentration while stirring blasts from container bottom equably, mixed gas flow is 120mL/min, and active carbon is carried out to surface oxidation reaction 1.5h;
(3) after reaction finishes, active carbon is taken out, use distilled water flushing post-drying, be cooled to room temperature, make the modified activated carbon for fuel desulfuration.
(1) Activated Carbon Pretreatment: active carbon washs to remove the inorganic and organic impurities of activated carbon surface successively through 0.1mol/L hydrochloric acid, 0.1mol/L NaOH and deionized water, at 110 ℃, dry standby after 2 hours;
(2) in the container of 100mL, add 30mL20 ℃ of distilled water, then by the NaOH solution adjusting pH value of 20 ℃ of 3mol/L, be 14.3, then add the pretreated active carbon of 1g, at ambient temperature, ozone-the air gas mixture that is 60mg/L by ozone concentration while stirring blasts from container bottom equably, mixed gas flow is 60mL/min, and active carbon is carried out to surface oxidation reaction 0.8h;
(3) after reaction finishes, active carbon is taken out, use distilled water flushing post-drying, be cooled to room temperature, make the modified activated carbon for fuel desulfuration.
embodiment 5
(1) Activated Carbon Pretreatment: active carbon washs to remove the inorganic and organic impurities of activated carbon surface successively through 0.1mol/L hydrochloric acid, 0.1mol/L NaOH and deionized water, at 110 ℃, dry standby after 2 hours;
(2) in the container of 100mL, add 18mL25 ℃ of distilled water, then by the NaOH solution adjusting pH value of 25 ℃ of 1mol/L, be 12.3, then add the pretreated active carbon of 1g, at ambient temperature, ozone-the air gas mixture that is 65mg/L by ozone concentration while stirring blasts from container bottom equably, mixed gas flow is 80mL/min, and active carbon is carried out to surface oxidation reaction 2h;
(3) after reaction finishes, active carbon is taken out, use distilled water flushing post-drying, be cooled to room temperature, make the modified activated carbon for fuel desulfuration.
(1) Activated Carbon Pretreatment: active carbon washs to remove the inorganic and organic impurities of activated carbon surface successively through 0.1mol/L hydrochloric acid, 0.1mol/L NaOH and deionized water, at 110 ℃, dry standby after 2 hours;
(2) in the container of 100mL, add 25mL25 ℃ of distilled water, then by the NaOH solution adjusting pH value of 25 ℃ of 2.5mol/L, be 14.3, then add the pretreated active carbon of 1g, at ambient temperature, ozone-the air gas mixture that is 15mg/L by ozone concentration while stirring blasts from container bottom equably, mixed gas flow is 120mL/min, and active carbon is carried out to surface oxidation reaction 3h;
(3) after reaction finishes, active carbon is taken out, use distilled water flushing post-drying, be cooled to room temperature, make the modified activated carbon for fuel desulfuration.
Modified activated carbon surface acid base groups concentration with Boehm titration measuring embodiment 1 ~ 6 preparation.Assay method is: take the tool plug conical flask that 0.5g sample is put into 100mL, the standard NaOH solution with deionized water preparation 0.1mol/L, pipettes 25mL alkali lye in conical flask with pipette, with High Purity Nitrogen stripping, further removes the CO in solution
2, be placed in the 24h that vibrates at 25 ℃ of constant temperature oscillation beds, measure supernatant liquor 10mL, add 40mL without CO
2water, with the hydrochloric acid solution of the 0.1mol/L of standard, carry out titration, record the variation of NaOH amount before and after vibration, the NaOH amount that the sample of unit of account quality consumes, as the quantity of its surface acidity functional group.
Measurement result is as shown in table 1, and the total surface acidity of known modified activated carbon is compared with original activity charcoal, obviously improves.
Acidic-group total content (the unit: mmol/g) of the modified active carbon surface of table 1 embodiment 1 ~ 6 preparation
Application Static Adsorption phase equilibrium experiment, the adsorption isotherm of the modified activated carbon of mensuration embodiment 1 ~ 6 preparation to thiophenic sulfur compound.Assay method is: under room temperature, prepare that initial sulphur concentration is respectively 0.5,1,3,6,8, the thiophene normal octane solution of 10mmol/L, then weigh respectively 0.1g modified activated carbon in 25mL conical flask, measure successively the thiophene solution of 5mL variable concentrations in each conical flask, as for shaking 24h in isothermal vibration bed, make it reach adsorption equilibrium, Temperature Setting is 30 ℃.The liquid equilibrium concentration of organic thiophenic sulfur in each sample of liquid-phase chromatographic analysis
c i *, the equilibrium adsorption capacity on unit adsorbent
q i computing formula is as follows:
The serial liquid equilibrium concentration recording according to experiment
c i *, calculate the adsorbance on corresponding serial unit adsorbent
q i, the mmol/kg of unit, with
q i ~ c i *mapping, just can draw the adsorption isotherm of organic thiophenic sulfur on active carbon.Isothermal height has reflected the adsorption capacity of this adsorbent to thiophenic sulfur compound.
The measurement result of embodiment 1 ~ 3 as shown in Figure 1.As shown in Figure 1, modified activated carbon to the adsorption isotherm of thiophenic sulfur compound apparently higher than original activity charcoal the adsorption isotherm to thiophenic sulfur compound.At 30 ℃, when equilibrium concentration is 9mmol/L, original activity charcoal is 42.4mmol/kg to the adsorbance of thiophene, and the equilibrium adsorption capacity of the modified activated carbon of embodiment 1 preparation is 48.2mmol/kg, the equilibrium adsorption capacity of the modified activated carbon of embodiment 2 preparations is 60.14mmol/kg, and the equilibrium adsorption capacity of the modified activated carbon of embodiment 3 preparations is 65.09mmol/kg.
The measurement result of embodiment 4 ~ 6 as shown in Figure 2.As shown in Figure 2, modified activated carbon to the adsorption isotherm of thiophenic sulfur compound apparently higher than original activity charcoal the adsorption isotherm to thiophenic sulfur compound.At 30 ℃, when liquid equilibrium concentration is 9mmol/L, original activity charcoal is 42.4mmol/kg to the adsorbance of thiophene, and the equilibrium adsorption capacity of the modified activated carbon of embodiment 4 preparations is 62.3mmol/kg, the equilibrium adsorption capacity of the modified activated carbon of embodiment 5 preparations is 69.1mmol/kg, and the equilibrium adsorption capacity of the modified activated carbon of embodiment 6 preparations is 79.1mmol/kg.
Claims (4)
1. for a preparation method for the modified activated carbon of fuel desulfuration, it is characterized in that, comprise the following steps:
(1) in reactor, add distilled water, adding sodium hydroxide solution to regulate pH value is 6.8 ~ 14.3, then adds active carbon, passes into while stirring the mist of ozone and air, and active carbon is carried out to surface oxidation reaction;
(2) after above-mentioned reaction finishes, active carbon is taken out, use distilled water flushing post-drying, be cooled to room temperature, make the modified activated carbon for fuel desulfuration.
2. preparation method according to claim 1, is characterized in that, in step (1), the molar concentration of described sodium hydroxide solution is 1 ~ 5mol/L; The temperature of described distilled water and sodium hydroxide solution is 15 ~ 35 ℃; The mass volume ratio of described active carbon and distilled water is 1:(10 ~ 30) g/mL.
3. preparation method according to claim 2, is characterized in that, in step (1), in described mist, the mass body volume concentrations of ozone is 15 ~ 65mg/L; The flow of described mist is 60 ~ 120mL/min.
4. modified activated carbon claimed in claim 1 is for adsorbing organic thiophenic sulfur of fuel oil.
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Cited By (7)
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| CN104587955A (en) * | 2014-12-30 | 2015-05-06 | 广东中烟工业有限责任公司 | Method for modifying tobacco activated carbon by virtue of ozone and application of modified activated carbon |
| CN105368492A (en) * | 2014-08-25 | 2016-03-02 | 青岛鑫润土苗木专业合作社 | High-efficiency and environmental-friendly gasoline desulphurization method |
| CN105964219A (en) * | 2016-05-11 | 2016-09-28 | 上海应用技术学院 | Method for optimizing adsorption of activated carbon to sulphur compounds in fuel oil |
| CN106367100A (en) * | 2016-09-05 | 2017-02-01 | 山东大学 | Method for one-step oxidation adsorption desulfurization by using nano carbon material and air oxygen |
| CN108906138A (en) * | 2018-07-04 | 2018-11-30 | 成都恩承科技股份有限公司 | A kind of regeneration method of active carbon or carbon-supported catalysts |
| CN109437189A (en) * | 2018-12-14 | 2019-03-08 | 科盛环保科技股份有限公司 | A kind of preparation of resin based sphere active carbon and application method |
| CN110467183A (en) * | 2019-09-09 | 2019-11-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Efficiently preparation process of column-shaped active carbon of removal benzene in air and products thereof and application |
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Cited By (8)
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|---|---|---|---|---|
| CN105368492A (en) * | 2014-08-25 | 2016-03-02 | 青岛鑫润土苗木专业合作社 | High-efficiency and environmental-friendly gasoline desulphurization method |
| CN104587955A (en) * | 2014-12-30 | 2015-05-06 | 广东中烟工业有限责任公司 | Method for modifying tobacco activated carbon by virtue of ozone and application of modified activated carbon |
| CN105964219A (en) * | 2016-05-11 | 2016-09-28 | 上海应用技术学院 | Method for optimizing adsorption of activated carbon to sulphur compounds in fuel oil |
| CN105964219B (en) * | 2016-05-11 | 2018-07-31 | 上海应用技术学院 | A kind of optimization method for sulphur compound in activated carbon adsorption fuel oil |
| CN106367100A (en) * | 2016-09-05 | 2017-02-01 | 山东大学 | Method for one-step oxidation adsorption desulfurization by using nano carbon material and air oxygen |
| CN108906138A (en) * | 2018-07-04 | 2018-11-30 | 成都恩承科技股份有限公司 | A kind of regeneration method of active carbon or carbon-supported catalysts |
| CN109437189A (en) * | 2018-12-14 | 2019-03-08 | 科盛环保科技股份有限公司 | A kind of preparation of resin based sphere active carbon and application method |
| CN110467183A (en) * | 2019-09-09 | 2019-11-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Efficiently preparation process of column-shaped active carbon of removal benzene in air and products thereof and application |
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Application publication date: 20140312 |