CN105132014B - The method that multiple biological activities agent is applied to coker gas oil desulfurization - Google Patents
The method that multiple biological activities agent is applied to coker gas oil desulfurization Download PDFInfo
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Abstract
The invention belongs to coker gas oil technical field of desulfurization, the method that multiple biological activities agent is applied to coker gas oil desulfurization is disclosed, is comprised the following steps：（1）Choline inositol composite powder or choline inositol composite sheet are added in coker gas oil, with heating and stirring in magnetic stirring apparatus, 60-100min is reacted, taking-up is cooled to room temperature；（2）Insulin is added in coker gas oil, heated at constant temperature in water bath with thermostatic control environment is subsequently placed in and stirs；（3）Cholic acids activating agent is added in coker gas oil, heated at constant temperature in water bath with thermostatic control environment is subsequently placed in and stirs 1-24 hours；（4）Catalyst and oxidant are successively added in coker gas oil, 50-100min of catalytic oxidation；（5）Add extractant at 1: 1 by volume, with 5-10min of magnetic stirrer, then pour into separatory funnel, stand 20min, collect diesel oil layer.The method desulfuration purification reaction condition of the present invention is gentle, environmental protection, and desulfurization degree is high, and coker gas oil yield is notable and the shallow taste of color is light.
Description
Technical field
The present invention relates to a kind of coker gas oil desulfurization technology, and in particular to the method for the coker gas oil desulfurization of high desulfurization rate.
Background technology
With the enhancing of people's environmental consciousness, people require increasingly strict to sulfur content of fuel oil standard, and countries in the world are equal
More strict new regulation has been formulated for the sulfur content in fuel oil.U.S.'s regulation diesel oil sulfur content in 2006 is by 500 μ g/g
It is reduced to 15 μ g/g；And Europe had been carried out the μ g/g of sulfur content 10 Europe V standards in 2009；Japan is the advanced of production clean gasoline
Country, the performed gasoline standards of JISK 2202 regulation, Japanese gasoline standard limitation sulfur content is 50ppm within 2005, and in
The national super low-sulfur oil standard that sulfur content is 10ppm of seeking unity of action in 2009.In China, derv fuel and gasoline were in 2005
European quality standard is implemented integrally from July 1,2010 are all up to standard, the sulfur content in regulation gasoline is less than 150 μ g/g,
Sulfur content in diesel oil is less than 350 μ g/g.Some line cities such as Beijing, Shanghai, Guangzhou perform the quasi- IV of Europe superscript, regulation gasoline and
Sulfur content in diesel oil is less than 50 μ g/g.And it is current, it is newest that " standard of state five " is by sulfur content index limits by fourth stage
50ppm is reduced to 10ppm, reduces 80%, implements in Beijing and Shanghai at present, before the end of the year 2017, and whole nation supply meets " state
Automobile-used vapour, the diesel oil of five " standards.Therefore, it can be said that domestic vehicle fuel will enter low-sulfur epoch of the sulfur content less than 50 μ g/g.
In face of increasingly strict sulfur content of fuel oil standard and market to the great demand of low-sulfur clean fuel oil, various countries are caused to cause one after another
Power is in the research of various desulfurization technologies.
With deepening continuously for Petroleum Processing Technology, an important deep working method of residual oil is to carry out coking, main at present
There are two kinds of autoclave coking and delayed coking.Coker gas oil is that residual oil passes through the product that coking is obtained.Coker gas oil is at me
Occupy sizable ratio in the finished diesel fuel yield of state, account for the 10% of light diesel fuel yield.Without refined coker gas oil matter
Amount is poor, not only black but also smelly containing non-hydrocarbon compounds such as substantial amounts of unsaturated hydrocarbons, more sulphur, nitrogen, oxygen, and the stability of diesel oil
Difference, gum level are high, colourity and insolubles content are higher.Substantial amounts of analysis and research show, the sulfur-containing compound in coker gas oil
Mainly there are elementary sulfur, hydrogen sulfide, mercaptan, thioether, thiophene, benzothiophene (BT), dibenzothiophenes (DBT) etc..Wherein, thiophene-based
Sulphur compound accounts for more than the 85% of coker gas oil total sulfur, and BT and DBT account for more than the 70% of thiophene-based.Therefore, thiophene-based is studied
Emphasis of the removing as desulfurizing oil of sulfide.Wherein elementary sulfur, hydrogen sulfide, mercaptan isoreactivity sulphur compound, set to oil refining
Have stronger corrosion failure effect.Elementary sulfur is a kind of 113 DEG C of fusing point, solid that is water insoluble and being dissolved in organic solvent,
There is good solvability in gasoline, but temperature is when being higher than 115 DEG C, can generate new sulfide and sulphur with some hydrocarbon reactions
Change hydrogen；Hydrogen sulfide is gas colourless and with rotten egg smell, and severe toxicity is slightly dissolved in water, is soluble in oil product, there is very strong reduction
Ability and corrosive power, the hydrosulphuric acid formed in water are weak binary acid.Mercaptan includes alkyl hydrosulfide, cycloalkyl mercaptan and aryl
Mercaptan, boiling point and water solubility are lower than the alcohol of same carbon number, are soluble in ethanol and ether.Mercaptan except there is disgusting foul smell,
Or a kind of oxidation inducing agent, makes the unstable component accelerated oxidation in gasoline and generates colloid, so that quality of gasoline becomes
Difference.Although the inactive sulfur such as thioether and thiophene compound corrodes relatively low to refining equipment, corrosion can be generated in combustion
Property very strong material.The characteristics of disulphide and polysulfide, is constantly declined with the increase stability of number of sulfur atoms, chemistry
Activity is continuously increased.When number of sulfur atoms is more than more than 3, its property and elementary sulfur are close.Heat is easily decomposed to thioether, list
Matter sulphur, mercaptan and alkene.Directly using for these diesel oil, China is not met not only the sulfur content in fuel oil is provided, and sternly
Heavily contaminated environment, it is serious to threaten the mankind's healthy.Therefore, coker gas oil must refine rear and can be used.
At present, the desulfurization technology of domestic and international fuel oil is broadly divided into hydrodesulfurization technology and non-hydrodesulfurization two is big
Class.Hydrodesulfurization technology produces low-sulfur diesel-oil, coker gas oil sulphur, nitrogen and colloid equal size can be greatly lowered, desulfurized effect is good,
Obtain meeting the fine-quality diesel oil of national standard；But it is due to that investment is big, high processing costs (180 yuan/t) are general only in large-scale refining
It is used widely in oily factory, and middle-size and small-size oil plant not only limited fund, moreover, hydrogen source is not enough, limits this method in
The application of little refinery plant.
Non-hydrodesulfurizationof of Diesel Fuel Refining is mainly de- including absorption desulfurization, abstraction desulfurization, complexing desulfurization, biological desulphurization, oxidation
Sulphur etc..The fuel oil of traditional acid-alkali refining method processing is extremely difficult to new low sulphur specifications, also technique exist in itself pollution,
The problems such as seriously corroded.Because bioanalysis desulfurization technology is not solved preferably the problem of in terms of rate of sulphur expulsion and stability
Certainly, so bioanalysis desulfurization also fails to embody its clear superiority；Catalytic oxidation desulfurization technology is gently produced because of its operating condition
Cost is relatively low, is welcome by middle-size and small-size oil plant very much.Therefore, the research of coker gas oil Desulfurization Technology is carried out, exploitation is a kind of new
Non- hydrodesulfurization refine coker gas oil method it is imperative.
Wherein, oxidation sweetening (ODS) technology reaction condition is gentle, technique is simple, non-hydrogen is operated, operating cost is low, safety
Environmental protection, equipment investment is few, also has higher desulfuration efficiency to the oil-source rock correlation that catalytic hydrogenation is difficult to remove, can reach
To the requirement of ultra-deep desulfurization, so that oxidizing process is referred to as green desulfurization technique geared to the 21st century, it is new as one in recent years
Study hotspot.Oxidation sweetening refer to strong oxidizer act under, the relatively low thioether of polarity and thiophene-based sulfur-bearing chemical combination in oil product
Thing is oxidized to the higher sulfoxide and sulfone compound of polarity, and these sulfide absorb oxygen atom and add dipole moment, so as to increase
The dissolubility in polar solvent is added, then has been removed by solvent extraction, to reach desulfurization purpose.At present, selective oxygen
Change desulfurization technology gentle with its process conditions, the features such as desulfurized effect is obvious receives the very big concern of oil refining industry.
Presently used oxidant mainly has hydrogen peroxide, O in the catalytic oxidation process of coker gas oil3, air, oil-soluble
Oxidant etc.；The use of organic acid, inorganic heteropolyacid, light or metal oxide etc. is catalyst；In order to improve desulfuration efficiency, also tie
Unify a little supplementary means and carry out oxidation sweetening, such as ultrasound oxidation technology method, plasma oxidation.By the sulfide in diesel oil through oxygen
Metaplasia into sulfone and sulfoxide by extract removing during, conventional extractant mainly has dimethyl sulfoxide, acetonitrile, N- methyl pyrroles
Pyrrolidone (NMP), DMF (DMF), furfural, nitromethane, ethylenediamine etc., research show these organic solvents
It is similar to sulfone class polarity, the sulfone class extract and separate in diesel oil after oxidation can be come out well.It is widely studied both at home and abroad at present
Oxidative desulfurization techniques mainly include hydrogen peroxide oxidation desulfurization, Oxygen Catalytic Oxidation desulfurization, ultrasound oxidation technology desulfurization and photochemistry oxygen
Change desulfurization etc., wherein because of H2O2Have the advantages that oxidisability is strong, oxidation Decomposition thing receives much concern to environment non-hazardous, it is de- in oxidation
Using wider in sulphur research.
In recent years, Non-hydrogenation Desulfurization Technique of Fuel Oil is developed rapidly, and this method is the oxidation removal under conditions of catalyst
Thioether, mercaptan and thiophene sulfides in coker gas oil, produce excellent desulfurized effect, so as to reach decolouring, deodorization, take off
Slag, so as to improve the purpose of diesel oil stability, gentle operating condition, low production cost, environmentally friendly life in addition
Production process, increasingly pays close attention to by domestic and international researcher.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of desulfuration purification reaction condition is gentle, environmental protection, desulfurization degree
The method that the multiple biological activities agent high, coker gas oil yield is notable and the shallow taste of color is light is applied to coker gas oil desulfurization.
The present invention adopts the following technical scheme that solution above-mentioned technical problem：
The method that multiple biological activities agent is applied to coker gas oil desulfurization, comprises the following steps：
(1), pre-process：Choline inositol composite powder or composite sheet are added in coker gas oil by 0.04-0.1g/ml, courage
Choline and inositol mass ratio respectively account for 50% in alkali inositol composite powder or composite sheet, are heated and stirred with magnetic stirring apparatus, and temperature is
36 DEG C -38 DEG C, speed of agitator is 20rpm, is reacted 1-24 hours；
(2), Cholic acids activating agent is added to step (1) as 0.05-1.0mg/ml obtained by coker gas oil in, then put
Heated at constant temperature is stirred in water bath with thermostatic control environment, and heating-up temperature is 36.5 DEG C -38 DEG C, heating response 1-24 hours, speed of agitator
For 20-40rpm；
(3), insulin is added in the coker gas oil obtained by step (2), constant temperature in water bath with thermostatic control environment is subsequently placed in
Heating stirring, heating-up temperature is 36.5-38 DEG C, heating response 1-24 hours, and speed of agitator is 20-40rpm；The insulin is
Powder ampoule agent for injection insulin or injection shape insulin, the addition of powder ampoule agent for injection insulin is 0.01-0.10mg/
ml；The volume ratio of injection shape insulin and coker gas oil is 2: 100-5: 100；
(4), catalyst and oxidant are successively added in the coker gas oil after step (3) processing, catalyst is trichlorine
Acetic acid or formic acid, oxidant are the hydrogenperoxide steam generators that mass concentration is 30%；The volume of coker gas oil, catalyst and oxidant
Than for 10: 2: 1-10: 4: 4, catalytic oxidation being carried out in magnetic stirring apparatus, the reaction time is 50-100min, and temperature is 50
DEG C -80 DEG C, mixing speed is 40rpm；
(5), extractant is added at 1: 1 by volume, extractant is DMF or furfural, uses magnetic stirring apparatus
5-10min is stirred, mixing speed is 40rpm, then pour into separatory funnel, stand 20min, collect diesel oil layer.
Cholic acids activator in the step (2) is cholic acid, cholate, deoxycholate, Ursodeoxycholic Acid Tablets, bear go
Oxycholic acid capsule, urso soft capsule, deoxycholic acid, hyodesoxycholic acid or glycocholic acid.
The choline inositol composite powder or choline or Choline Chloride in composite sheet.
The water bath with thermostatic control environment of the step (2) and step (3) uses water bath with thermostatic control magnetic stirring apparatus, and power is 40w.
Compared with prior art, the advantage of the invention is that：
1st, technological process is simple, and operation is simple；
2nd, this method is applied to coker gas oil desulfuration purification reaction condition gently, and environmental protection, desulfurized effect is substantially, limpid
Transparent light yellow diesel yield is notable.
Embodiment
Below in conjunction with embodiment to the detailed description of the invention, but do not constitute to the claims in the present invention protection domain
Limitation.
Embodiment 1：
Weigh 0.4g choline inositol composite powders to be added in 10ml coker gas oils, choline and inositol in choline inositol composite powder
Mass ratio respectively accounts for 50%, is put into together in beaker, is placed in DF-101S instant-heating-type constant-temperatures heating magnetic stirring apparatus, temperature is 36
DEG C, speed of agitator is 20rpm, and reaction is pre-processed for 1 hour.Insulin is added in above-mentioned coker gas oil under normal temperature, pancreas
Island element is powder ampoule agent for injection insulin, and its addition is 0.01mg/ml, is subsequently placed in heated at constant temperature in water bath with thermostatic control environment and stirs
Mix, heating-up temperature is 36.5 DEG C, heating response 1 hour, the power of the magnetic stirring apparatus of constant temperature is 40w, and rotating speed is 20-40rpm；
Cholic acid is added in above-mentioned coker gas oil by 0.05mg/ml under normal temperature, is subsequently placed in heated at constant temperature in water bath with thermostatic control environment
Stirring, heating-up temperature is 36.5 DEG C, and heating response 1 hour, water bath with thermostatic control environment uses water bath with thermostatic control magnetic stirring apparatus, power
For 40w, rotating speed is 20rpm；Catalyst and oxidant are successively added in gained coker gas oil, catalyst is trichloroacetic acid,
Oxidant is the hydrogenperoxide steam generator that mass concentration is 30%；Coker gas oil, catalyst and oxidant volume ratio are 10: 2: 1, then
Catalytic oxidation is carried out in DF-101S heat collecting type constant-temperature heating magnetic stirring apparatus, the reaction time is 50min, heating-up temperature
For 50 DEG C, mixing speed is 40rpm；Then, coker gas oil is taken out, be cooled to after room temperature, add extractant N, N- diformazan
The volume ratio of base formamide, extractant and coker gas oil is 1: 1, then uses magnetic stirrer 5min, and mixing speed is
40rpm, then separatory funnel is poured into, 20min is stood, diesel oil layer is collected, and its volume is measured, diesel yield is obtained, by collection
It is 0.00513% that diesel oil, which measures sulfur content with Sinie7039XR Single wavelength X-fluorescence sulphur content analyzer, and abstraction desulfurization rate is
98.18%, diesel yield is 81%.
Embodiment 2：
Weigh 0.6g choline inositol composite sheets to be added in 10ml coker gas oils, choline or Choline Chloride and flesh in composite sheet
Alcohol mass ratio respectively accounts for 50%, is put into together in beaker, is placed in DF-101S instant-heating-type constant-temperatures heating magnetic stirring apparatus, temperature is
37 DEG C, speed of agitator is 20rpm, and reaction is pre-processed for 8 hours.Insulin is added under normal temperature above-mentioned coker gas oil
In, insulin is injection shape insulin, and the volume ratio of insulin and coker gas oil is 3: 100, is subsequently placed in water bath with thermostatic control ring
Heated at constant temperature is stirred in border, and heating-up temperature is 37 DEG C, heating response 15 hours, and the power of the magnetic stirring apparatus of constant temperature is 40w, is turned
Speed is 30rpm；Sodium taurocholate is added in coker gas oil by 0.5mg/ml under normal temperature, constant temperature in water bath with thermostatic control environment is subsequently placed in
Heating stirring, heating-up temperature is 37 DEG C, and heating response 15 hours, water bath with thermostatic control environment uses water bath with thermostatic control magnetic stirring apparatus,
Power is 40w, and rotating speed is 30rpm；Catalyst and oxidant are successively added in above-mentioned coker gas oil, catalyst is first
Acid, oxidant is the hydrogenperoxide steam generator that mass concentration is 30%；Coker gas oil, catalyst and oxidant volume ratio are 10: 2.5
: 2, it is placed in DF-101S heat collecting type constant-temperature heating magnetic stirring apparatus and carries out catalytic oxidation, the reaction time is 70min, heats
Temperature is 60 DEG C, and mixing speed is 40rpm；Then, coker gas oil is taken out, is cooled to after room temperature, add extractant furfural,
The volume ratio of extractant and coker gas oil is 1: 1, then uses magnetic stirrer 7min, mixing speed, is that 40rpm is poured into point again
Liquid funnel, stands 20min, collects diesel oil layer, and measures its volume, obtains diesel yield, the diesel oil of collection is used
It is 0.00436% that Sinie7039XR Single wavelength X-fluorescence sulphur content analyzer, which measures its sulfur content, and abstraction desulfurization rate is 98.95%, bavin
Oil yield is 82%.
Embodiment 3：
Weigh 0.8g choline inositol composite powders to be added in 10ml coker gas oils, choline and inositol mass ratio are each in composite powder
50% is accounted for, is put into together in beaker, is placed in DF-101S instant-heating-type constant-temperatures heating magnetic stirring apparatus, temperature is 37.5 DEG C, stirring
Rotating speed is 20rpm, and reaction is pre-processed for 16 hours.Insulin is added in above-mentioned coker gas oil under normal temperature, insulin
For injection shape insulin, the volume ratio of insulin and coker gas oil is 4: 100, is subsequently placed in constant temperature in water bath with thermostatic control environment and adds
Thermal agitation, heating-up temperature is 37.5 DEG C, heating response 20 hours, and the power of the magnetic stirring apparatus of constant temperature is 40w, and rotating speed is
35rpm；Ursodeoxycholic Acid Tablets are added in coker gas oil by 0.7mg/ml under normal temperature, are subsequently placed in water bath with thermostatic control environment permanent
Warm heating stirring, heating-up temperature is 37.5 DEG C, and heating response 20 hours, water bath with thermostatic control environment uses water bath with thermostatic control magnetic agitation
Device, power is 40w, and rotating speed is 35rpm；Catalyst and oxidant are successively added in coker gas oil, catalyst is three chloroethenes
Acid, oxidant is the hydrogenperoxide steam generator that mass concentration is 30%；Coker gas oil, catalyst and oxidant volume ratio are 10: 3:
3, then catalytic oxidation is carried out in DF-101S heat collecting type constant-temperature heating magnetic stirring apparatus, the reaction time is 90min, heating
Temperature is 70 DEG C, and mixing speed is 40rpm；Then, coker gas oil is taken out, be cooled to after room temperature, add extractant N, N-
Dimethylformamide, extractant is 1: 1 with coker gas oil volume ratio, then uses magnetic stirrer 8min, and mixing speed is
40rpm, then separatory funnel is poured into, 20min is stood, diesel oil layer is collected, and its volume is measured, diesel yield is obtained, by collection
It is 0.00376% that diesel oil, which measures its sulfur content with Sinie7039XR Single wavelength X-fluorescence sulphur content analyzer, and abstraction desulfurization rate is
99.55%, diesel yield is 85%.
Embodiment 4：
Weigh 1.0g choline inositol composite sheets to be added in 10ml coker gas oils, choline and inositol mass ratio are each in composite sheet
50% is accounted for, is put into together in beaker, is placed in DF-101S instant-heating-type constant-temperatures heating magnetic stirring apparatus, temperature is 38 DEG C, and stirring turns
Speed is 20rpm, and reaction is pre-processed for 24 hours.Insulin is added in above-mentioned coker gas oil under normal temperature, insulin is
Powder ampoule agent for injection insulin, its addition is 0.1mg/ml, is subsequently placed in heated at constant temperature in water bath with thermostatic control environment and stirs, heating
Temperature is 38 DEG C, and heating response 24 hours, water bath with thermostatic control environment uses water bath with thermostatic control magnetic stirring apparatus, and power is 40w, rotating speed
For 40rpm；Deoxycholic acid is added in foregoing coker gas oil by 1mg/ml under normal temperature, be subsequently placed in water bath with thermostatic control environment
Heated at constant temperature is stirred, and heating-up temperature is 38 DEG C, and heating response 24 hours, water bath with thermostatic control environment uses water bath with thermostatic control magnetic agitation
Device, power is 40w, and rotating speed is 40rpm；Catalyst and oxidant are successively added in coker gas oil, catalyst is three chloroethenes
Acid, oxidant is the hydrogenperoxide steam generator that mass concentration is 30%；Coker gas oil, catalyst and oxidant volume ratio are 10: 4:
4, then catalytic oxidation is carried out in DF-101S heat collecting type constant-temperature heating magnetic stirring apparatus, the reaction time is 100min, heating
80 DEG C of temperature, mixing speed is 40rpm；Then, coker gas oil is taken out, be cooled to after room temperature, add extractant furfural, extracted
The volume ratio for taking agent and coker gas oil is 1: 1, then uses magnetic stirrer 10min, mixing speed is 40rpm, then is poured into point
Liquid funnel, stands 20min, collects diesel oil layer, and measures its volume, obtains diesel yield, the diesel oil of collection is used
It is 0.00348% that Sinie7039XR Single wavelength X-fluorescence sulphur content analyzer, which measures its sulfur content, and abstraction desulfurization rate is 99.83%, bavin
Oil yield is 89%.
Claims (3)
1. the method that multiple biological activities agent is applied to coker gas oil desulfurization, it is characterised in that comprise the following steps：
（1）, pretreatment：Choline inositol composite powder or composite sheet are added in coker gas oil by 0.04-0.1g/ml, choline flesh
Choline and inositol mass ratio respectively account for 50% in alcohol composite powder or composite sheet, are heated and stirred with magnetic stirring apparatus, temperature be 36 DEG C-
38 DEG C, speed of agitator is 20rpm, is reacted 1-24 hours；
（2）, by 0.05-1.0mg/ml Cholic acids activating agent is added to step（1）In the coker gas oil of gained, perseverance is subsequently placed in
Heated at constant temperature is stirred in tepidarium environment, and heating-up temperature is 36.5 DEG C-38 DEG C, heating response 1-24 hours, and speed of agitator is
20—40rpm；
（3）, insulin is added to step（2）In the coker gas oil of gained, heated at constant temperature in water bath with thermostatic control environment is subsequently placed in
Stirring, heating-up temperature is 36.5-38 DEG C, heating response 1-24 hours, and speed of agitator is 20-40rpm；The insulin is
Powder ampoule agent for injection insulin or injection shape insulin, the addition of powder ampoule agent for injection insulin is 0.01-0.10mg/
ml；The volume ratio of injection shape insulin and coker gas oil is 2:100—5:100；
（4）, catalyst and oxidant be successively added to step（3）In coker gas oil after processing, catalyst is trichloroacetic acid
Or formic acid, oxidant is the hydrogenperoxide steam generator that mass concentration is 30%；The volume ratio of coker gas oil, catalyst and oxidant is
10: 2: 1-10: 4: 4, catalytic oxidation is carried out in magnetic stirring apparatus, the reaction time is 50-100min, and temperature is 50
DEG C -80 DEG C, mixing speed is 40rpm；
（5）, 1: 1 addition extractant is to step by volume（4）In coker gas oil after processing, extractant is N, N- dimethyl methyls
Acid amides or furfural, with 5-10min of magnetic stirrer, mixing speed is 40rpm, then pours into separatory funnel, stands 20min,
Collect diesel oil layer.
2. the method that multiple biological activities agent according to claim 1 is applied to coker gas oil desulfurization, it is characterised in that institute
State step（2）In Cholic acids activating agent be cholic acid, cholate, deoxycholate, Ursodeoxycholic Acid Tablets, urso glue
Capsule, urso soft capsule, deoxycholic acid, hyodesoxycholic acid or glycocholic acid.
3. the method that multiple biological activities agent according to claim 1 is applied to coker gas oil desulfurization, it is characterised in that institute
State step（2）And step（3）Water bath with thermostatic control environment use water bath with thermostatic control magnetic stirring apparatus, power is 40w.
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