CN105112096A - Method of applying insulin to coking diesel oil desulfurization - Google Patents
Method of applying insulin to coking diesel oil desulfurization Download PDFInfo
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Abstract
The invention discloses a method of applying insulin to coking diesel oil desulfurization. The method comprises the following steps: (1) adding medicinal dried hawthorn powder or hawthorn water into coking diesel oil, heating and stirring in a magnetic stirring machine, conducting reaction for 60-100 min, taking out the coking diesel oil, and cooling to the room temperature; (2) adding insulin into the coking diesel oil obtained in the step (1) according to the mass-to-volume ratio of (0.05-1):1, then placing in a thermostatic water bath environment, heating at constant temperature while stirring for 1-24 h; (3) adding a catalyst and an oxidant into the coking diesel oil in sequence, and conducting catalytic oxidation reaction in the magnetic stirring machine for 50-100 min; (4) cooling to the room temperature, adding an extracting agent according to the volume ratio of 1:1, stirring in the magnetic stirring machine for 5-10 min, then pouring the mixture into a separating funnel, leaving the mixture to stand for 20 min, and collecting the diesel oil layer. According to the method, the reaction conditions of desulfurization and refining are mild, environment can be protected, the desulfurization rate is high, the yield of the coking diesel oil is obvious, and the color and smell of the coking diesel oil are light.
Description
Technical field
The present invention relates to coker gas oil desulfurization technology, be specifically related to the method for the coker gas oil desulfurization of high desulfurization rate.
Background technology
Along with the enhancing of people's environmental consciousness, people are increasingly strict to sulfur content of fuel oil standard-required, and comparatively strict new regulation has all been formulated for the sulphur content in oil fuel in countries in the world.U.S.'s regulation diesel oil sulphur content in 2006 reduces to 15 μ g/g by 500 μ g/g; And the Europe V standard of sulphur content 10 μ g/g has been implemented in Europe in 2009; Japan is the advanced country producing clean gasoline, performed JISK2202 gasoline standard regulation, and within 2005, Japanese gasoline standard restriction sulphur content is 50ppm, and national sulphur content of seeking unity of action was the super low-sulfur oil standard of 10ppm in 2009.In China, derv fuel oil and gasoline implemented integrally European quality standard in 1 day July in 2005, and 2010 all up to standard, and the sulphur content in regulation gasoline is less than 150 μ g/g, and the sulphur content in diesel oil is less than 350 μ g/g.Some line cities such as Beijing, Shanghai, Guangzhou perform Europe superscript accurate IV, and the sulphur content in regulation gasoline and diesel oil is less than 50 μ g/g.And at present, sulphur content index limits is reduced to 10ppm by the 50ppm of fourth stage by up-to-date " state five " standard, reduces 80%, implement in Beijing and Shanghai at present, before the end of the year 2017, whole nation supply meets automobile-used vapour, the diesel oil of " state five " standard.Therefore, domestic vehicle fuel will enter sulphur content and be less than the low-sulfur epoch of 50 μ g/g.In the 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 be devoted to the research of various desulfurization technology one after another.
Along with deepening continuously of Petroleum Processing Technology, an important deep processing method of residual oil carries out coking, mainly contains autoclave coking and delayed coking two kinds at present.Coker gas oil is the product that residual oil obtains through coking.Coker gas oil occupies sizable ratio in the finished diesel fuel output of China, accounts for 10% of solar oil output.Second-rate without refining coker gas oil, containing non-hydrocarbon compounds such as a large amount of unsaturated hydrocarbons, more sulphur, nitrogen, oxygen, not only black but also smelly, and the stability of diesel oil is poor, gum level is high, colourity and insolubles content higher.A large amount of analysis and research show, the sulfocompound in coker gas oil mainly contains elementary sulfur, hydrogen sulfide, mercaptan, thioether, thiophene, thionaphthene (BT), dibenzothiophene (DBT) etc.Wherein, thiophene sulphur compound accounts for more than 85% of coker gas oil total sulfur, and BT and DBT accounts for more than 70% of thiophene-based.Therefore, that studies thiophene-type sulfide removes the emphasis becoming desulfurizing oil.Wherein elementary sulfur, hydrogen sulfide, mercaptan isoreactivity sulphur compound, have stronger corrosion failure effect to refining equipment.Elementary sulfur is a kind of fusing point 113 DEG C, water insoluble and be dissolved in the solid of organic solvent, have good dissolving power in the oil, but temperature higher than 115 DEG C time, can with some hydrocarbon reaction, generate new sulfide and hydrogen sulfide, hydrogen sulfide is colourless and has the gas of rotten egg smell, severe toxicity, slightly water-soluble, be soluble in oil product, have very strong reducing power and corrosive power, the hydrosulphuric acid formed in water is weak diprotic acid.Mercaptan comprises alkyl sulfhydryl, cycloalkyl mercaptan and aryl mercaptan, boiling point and water-soluble ratio low with the alcohol of carbon number, be soluble in ethanol and ether.Mercaptan is except there being disgusting foul smell, or a kind of oxidation inducer, makes the unstable component accelerated oxidation in gasoline and generates colloid, thus quality of gasoline is deteriorated.Although the inactive sulfur such as thioether and thiophene compound is lower to refining equipment corrosion, the very strong material of corrodibility can be generated in combustion.The feature of disulphide and polysulfide is that chemically reactive constantly increases along with the increase stability of number of sulfur atoms constantly declines.When number of sulfur atoms is greater than more than 3, its character is close with elementary sulfur.Heat is easily decomposed into thioether, elemental sulfur, mercaptan and alkene.The direct use of these diesel oil, does not only meet China to the sulphur content regulation in oil fuel, and serious environment pollution, the serious threat mankind's is healthy.Therefore, coker gas oil can use after must refining.
At present, the desulfurization technology of domestic and international oil fuel is mainly divided into hydrogenating desulfurization technology and the large class of non-hydrodesulfurization two, hydrogenating desulfurization technology produces low-sulfur diesel-oil, significantly can reduce coker gas oil sulphur, nitrogen and colloid equal size, sweetening effectiveness is good, the fine-quality diesel oil obtaining meeting national standard is still large owing to investing, tooling cost high (180 yuan/t), be used widely in Large-scale Refinery for general, and middle-size and small-size refinery not only limited fund, moreover hydrogen source is not enough, limits the application of the method at middle-size and small-size refinery.Non-hydrodesulfurizationof of Diesel Fuel Refining mainly comprises adsorption desulfurize, abstraction desulfurization, complexing desulfurization, biological desulphurization, oxidation sweetening etc.The fuel oil of traditional acid-alkali refining method process is difficult to reach new low sulphur specifications, moreover technique itself also exists the problems such as pollution, seriously corroded; Because the problem of biological process desulfurization technology in desulfurization rate and stability is not solved preferably, so biological process desulfurization also fails to embody its clear superiority; Catalytic oxidation desulfurization technology is lower with the gentle production cost of its operational condition, very by the welcome of middle-size and small-size refinery.Therefore, carry out the research of coker gas oil Desulfurization Technology, a kind of method developing non-hydrogenation desulfuration purification coker gas oil is newly imperative.
Wherein, oxidation sweetening (ODS) technology reaction conditions is gentle, technique is simple, non-hydrogen operates, process cost is low, safety and environmental protection, facility investment is few, also higher desulfuration efficiency is had to the oil-source rock correlation that shortening is difficult to remove, the requirement of ultra-deep desulfurization can be reached, thus oxidation style is called as green desulfurization technique geared to the 21st century, become a new study hotspot in recent years.Oxidation sweetening refers under strong oxidizer effect, the thioether that oil product Semi-polarity is lower and thiophene sulfocompounds are oxidized to the higher sulfoxide of polarity and sulfone compound, these sulfide absorbs Sauerstoffatom and adds moment of dipole, thus add the solvability in polar solvent, be removed by solvent extraction again, to reach desulfurization object.At present, selective oxidation desulfurization technology is gentle with its processing condition, and the features such as sweetening effectiveness is obvious, receive the very big concern of oil refining industry.
Oxygenant used at present in the catalytic oxidation process of coker gas oil mainly contains hydrogen peroxide, O
3, air, oil insoluble oxidation agent etc.; Organic acid, inorganic heteropolyacid, light or metal oxide etc. is used to be catalyzer; In order to improve desulfuration efficiency, also carry out oxidation sweetening in conjunction with some supplementary meanss, as ultrasound oxidation technology method, plasma oxidation etc.In the process removed the sulfone and sulfoxide of the sulfide in diesel oil through being oxidized generation by extraction, conventional extraction agent mainly contains methyl-sulphoxide, acetonitrile, N-Methyl pyrrolidone (NMP), N, dinethylformamide (DMF), furfural, Nitromethane 99Min., quadrol etc., research shows these organic solvents and sulfone class polar phase seemingly, can well by the sulfone class extracting and separating in diesel oil after oxidation out.The oxidative desulfurization techniques of extensively research both at home and abroad mainly comprises hydrogen peroxide oxidation desulfurization, Oxygen Catalytic Oxidation desulfurization, ultrasound oxidation technology desulfurization and Photochemical Oxidative Desulfurization of Fluidized etc., wherein because of H at present
2o
2have that oxidisability is strong, oxygenolysis thing receives much concern without advantages such as harm to environment, apply wider in oxidation sweetening is studied.
In recent years, Non-hydrogenation Desulfurization Technique of Fuel Oil develops rapidly, the method is under the condition of catalyzer, and the thioether in oxidation removal coker gas oil, mercaptan and thiophene sulfides, produce excellent sweetening effectiveness, thus reach decolouring, deodorization, de-slag, thus improve the object of diesel oil stability, in addition gentle operational condition, low production cost, environmentally friendly production process, more and more by the concern of being inside and outside investigator.
Summary of the invention
It is gentle that the technical problem to be solved in the present invention is to provide a kind of desulfuration purification reaction conditions, environmental protection, and desulfurization degree is high, and coker gas oil yield significantly and the light Regular Insulin of look shallow taste is applied to the method for coker gas oil desulfurization.
The present invention adopts following technical scheme to solve the problems of the technologies described above:
Regular Insulin is applied to the method for coker gas oil desulfurization, comprises the following steps:
(1), add in coker gas oil by 0.2-0.8g/ml by medicinal dry hawthorn fruit or hawthorn water, heat and stir with magnetic stirring apparatus, temperature is 40 DEG C-100 DEG C, and mixing speed is 20rpm, reaction 60-100min, then takes out and is cooled to room temperature;
(2), Regular Insulin add in the coker gas oil of step (1) gained, be then placed in water bath with thermostatic control environment thermostatically heating and stir, temperature is 36.5 DEG C-38 DEG C, reacting by heating 1-24 hour, and mixing speed is 20-40rpm; Described Regular Insulin is powder ampoule agent for injection Regular Insulin or injection shape Regular Insulin, and the addition of powder ampoule agent for injection Regular Insulin is 0.01-0.10mg/ml; The volume ratio of injection shape Regular Insulin and coker gas oil is 2: 100-5: 100;
(3), catalyzer and oxygenant successively add in the coker gas oil after step (2) process, catalyzer is trichoroacetic acid(TCA) or formic acid, oxygenant to be mass concentration be 30% superoxol; The volume ratio of coker gas oil, catalyzer and oxygenant is 10: 2: 1-10: 4: 4, in magnetic stirring apparatus, carry out catalytic oxidation, and the reaction times is 50-100min, and temperature is 50 DEG C-80 DEG C, and stirring velocity is 40rpm;
(4) after, step (3) gained coker gas oil is cooled to room temperature, add extraction agent at 1: 1 by volume, extraction agent is N, dinethylformamide or furfural, use magnetic stirrer 5-10min, stirring velocity is 40rpm, then pours separating funnel into, leave standstill 20min, collect diesel oil layer.
Hawthorn water in described step (1) is that water adds the hawthorn water obtained after medicinal dry hawthorn decocts 2 hours by 300ml/g.
Magnetic stirring apparatus in described step (1) and step (3) all adopts DF-101S instant-heating-type constant-temperature to heat magnetic stirring apparatus.
Described step (2) adopts water bath with thermostatic control magnetic stirring apparatus, and power is 40w.
Compared with prior art, the invention has the advantages that:
1, technical process is simple, and operation is simple;
2, the method is applied to coker gas oil desulfuration purification reaction conditions gentleness, and environmental protection, desulfurization degree is high, and as clear as crystal light yellow diesel yield is remarkable.
Embodiment
Below in conjunction with embodiment, the present invention is elaborated, but do not form the restriction to the claims in the present invention protection domain.
Embodiment 1:
Hawthorn is parts of generic medicinal plants, have another name called fruit, Fruit of Pashi Pear in mountain, Rosaceae defoliation small arbor, its fruit contains the chemical compositions such as flavonoid, flavanoid, triterpenes and organic acid, wherein Quercetin 3-galactoside, ursolic acid are the main components of flavonoid and triterpenes, are the activeconstituentss of Antilipemic haw.Hawthorn contains a large amount of tartaric acid, Crategolic acid, Citric Acid and lipase, lipolytic enzyme, can promote steatolysis, has the effect of cholesterol degradation and triglyceride level.In addition, also containing the organic amine chemical composition such as choline (choline), vagusstoff (acetylcholine), be also the effective constituent of lipopenicillinase.
Weigh the medicinal dry hawthorn fruit of 2g to add in 10ml coker gas oil, put into beaker together, and with in DF-101S instant-heating-type constant-temperature heating magnetic stirring apparatus, temperature is 40 DEG C, and mixing speed is 20rpm, and reaction 60min, rear taking-up is cooled to room temperature.Be 2: 100 injection shape Regular Insulin is added in coker gas oil by volume under normal temperature; Then be placed in water bath with thermostatic control environment thermostatically heating to stir, Heating temperature is 36.5 DEG C, reacting by heating 1 hour, and the power of the magnetic stirring apparatus of constant temperature is 40w, and rotating speed is 20rpm; Catalyzer and oxygenant are successively added in coker gas oil, and catalyzer is trichoroacetic acid(TCA), oxygenant to be mass concentration be 30% superoxol; Coker gas oil, catalyzer and oxygenant volume ratio are 10: 2: 1, then carry out catalytic oxidation with in DF-101S heat collecting type constant-temperature heating magnetic stirring apparatus, and the reaction times is 50min, and Heating temperature is 50 DEG C, and stirring velocity is 40rpm; Then, after coker gas oil taking-up is cooled to room temperature, then add extraction agent DMF, the volume ratio of extraction agent and coker gas oil is 1: 1, use magnetic stirrer 5min, stirring velocity is 40rpm, then pours separating funnel into, leave standstill 20min, collect diesel oil layer, and measure its volume, obtain diesel yield; It is 0.00634% that the diesel oil Sinie7039XR Single wavelength X-fluorescence sulphur content analyzer of collection is surveyed its sulphur content, and abstraction desulfurization rate is 97.70%, and diesel yield is 80%.
Embodiment 2:
Weigh the medicinal dry hawthorn fruit of 4g to add in 10ml coker gas oil, put into beaker together, and with in DF-101S instant-heating-type constant-temperature heating magnetic stirring apparatus, temperature is 60 DEG C, and mixing speed is 20rpm, and reaction 80min, rear taking-up is cooled to room temperature.Be the powder ampoule agent for injection Regular Insulin of 0.05mg/ml by addition under normal temperature, add in coker gas oil; Then be placed in water bath with thermostatic control environment thermostatically heating to stir, Heating temperature is 37 DEG C, reacting by heating 15 hours, and the power of the magnetic stirring apparatus of constant temperature is 40w, and rotating speed is 30rpm; Catalyzer and oxygenant are successively added in coker gas oil, and catalyzer is formic acid, oxygenant to be mass concentration be 30% superoxol; Coker gas oil, catalyzer and oxygenant volume ratio are 10: 2.5: 2, then carry out stirring catalytic oxidation with in DF-101S heat collecting type constant-temperature heating magnetic stirring apparatus, and the reaction times is 70min, and Heating temperature is 60 DEG C, and stirring velocity is 40rpm; After coker gas oil taking-up is cooled to room temperature, then add extraction agent furfural, the volume ratio of extraction agent and coker gas oil is 1: 1, then uses magnetic stirrer 7min, stirring velocity is 40rpm, then pours separating funnel into, leaves standstill 20min, collect diesel oil layer, and measure its volume, obtain diesel yield; It is 0.00585% that the diesel oil Sinie7039XR Single wavelength X-fluorescence sulphur content analyzer of collection is surveyed its sulphur content, and abstraction desulfurization rate is 98.19%, and diesel yield is 82%.
Embodiment 3:
Water adds after medicinal dry hawthorn decocts 2 hours by 300ml/g and obtains hawthorn water, 6g hawthorn water is added in 10ml coker gas oil, put into beaker together, and with in DF-101S instant-heating-type constant-temperature heating magnetic stirring apparatus, temperature is 80 DEG C, mixing speed is 20rpm, and reaction 90min, rear taking-up is cooled to room temperature.Be the powder ampoule agent for injection Regular Insulin of 0.08mg/ml by addition under normal temperature, add in coker gas oil; Then be placed in water bath with thermostatic control environment thermostatically heating to stir, Heating temperature is 37.5 DEG C, reacting by heating 20 hours, and the power of the magnetic stirring apparatus of constant temperature is 40w, and rotating speed is 35rpm; Catalyzer and oxygenant are successively added in coker gas oil, and catalyzer is trichoroacetic acid(TCA), oxygenant to be mass concentration be 30% superoxol; Coker gas oil, catalyzer and oxygenant volume ratio are 10: 3: 3, then carry out stirring catalytic oxidation with in DF-101S heat collecting type constant-temperature heating magnetic stirring apparatus, and the reaction times is 90min, and Heating temperature is 70 DEG C, and stirring velocity is 40rpm; Then, after coker gas oil taking-up is cooled to room temperature, then extraction agent N is added, dinethylformamide, extraction agent is 1: 1 with coker gas oil agent oil volume ratio, then uses magnetic stirrer 8min, stirring velocity is 40rpm, then pours separating funnel into, leaves standstill 20min, collect diesel oil layer, and measure its volume, obtain diesel yield, it is 0.00463% that the diesel oil Sinie7039XR Single wavelength X-fluorescence sulphur content analyzer of collection is surveyed its sulphur content, abstraction desulfurization rate is 98.68%, and diesel yield is 85%.
Embodiment 4:
Weigh the medicinal dry hawthorn fruit of 8g to add in 10ml coker gas oil, put into beaker together, and with in DF-101S instant-heating-type constant-temperature heating magnetic stirring apparatus, temperature is 100 DEG C, and mixing speed is 20rpm, and reaction 100min, rear taking-up is cooled to room temperature.Be 5: 100 injection shape Regular Insulin is added in coker gas oil by volume under normal temperature; Then be placed in water bath with thermostatic control environment thermostatically heating to stir, Heating temperature is 38 DEG C, reacting by heating 24 hours, and the power of the magnetic stirring apparatus of constant temperature is 40w, and rotating speed is 40rpm; Catalyzer and oxygenant are successively added in coker gas oil, and catalyzer is formic acid, oxygenant to be mass concentration be 30% superoxol; Coker gas oil, catalyzer and oxygenant volume ratio are 10: 4: 4, oxidizing temperature is 80 DEG C, and stirring velocity is 40rpm, then carries out catalytic oxidation with in DF-101S heat collecting type constant-temperature heating magnetic stirring apparatus, and the reaction times is 100min, Heating temperature 80 DEG C; After coker gas oil taking-up is cooled to room temperature, then add extraction agent furfural, extraction agent is 1: 1 with the agent oil volume ratio of coker gas oil, use magnetic stirrer 10min again, stirring velocity is 40rpm, then pours separating funnel into, leaves standstill 20min, collect diesel oil layer, and measure its volume, obtain diesel yield, it is 0.00402% that the diesel oil Sinie7039XR Single wavelength X-fluorescence sulphur content analyzer of collection is surveyed its sulphur content, abstraction desulfurization rate is 99.29%, and diesel yield is 87%.
Claims (4)
1. Regular Insulin is applied to the method for coker gas oil desulfurization, it is characterized in that, comprises the following steps:
(1), add in coker gas oil by 0.2-0.8g/ml by medicinal dry hawthorn fruit or hawthorn water, heat and stir with magnetic stirring apparatus, temperature is 40 DEG C-100 DEG C, and mixing speed is 20rpm, reaction 60-100min, then takes out and is cooled to room temperature;
(2), Regular Insulin add in the coker gas oil of step (1) gained, be then placed in water bath with thermostatic control environment thermostatically heating and stir, temperature is 36.5 DEG C-38 DEG C, reacting by heating 1-24 hour, and mixing speed is 20-40rpm; Described Regular Insulin is powder ampoule agent for injection Regular Insulin or injection shape Regular Insulin, and the addition of powder ampoule agent for injection Regular Insulin is 0.01-0.10mg/ml; The volume ratio of injection shape Regular Insulin and coker gas oil is 2: 100-5: 100;
(3), catalyzer and oxygenant successively add in the coker gas oil after step (2) process, catalyzer is trichoroacetic acid(TCA) or formic acid, oxygenant to be mass concentration be 30% superoxol; The volume ratio of coker gas oil, catalyzer and oxygenant is 10: 2: 1-10: 4: 4, in magnetic stirring apparatus, carry out catalytic oxidation, and the reaction times is 50-100min, and temperature is 50 DEG C-80 DEG C, and stirring velocity is 40rpm;
(4) after, step (3) gained coker gas oil is cooled to room temperature, add extraction agent at 1: 1 by volume, extraction agent is N, dinethylformamide or furfural, use magnetic stirrer 5-10min, stirring velocity is 40rpm, then pours separating funnel into, leave standstill 20min, collect diesel oil layer.
2. Regular Insulin according to claim 1 is applied to the method for coker gas oil desulfurization, it is characterized in that, the hawthorn water in described step (1) is that water adds the hawthorn water obtained after medicinal dry hawthorn decocts 2 hours by 300ml/g.
3. Regular Insulin according to claim 1 is applied to the method for coker gas oil desulfurization, it is characterized in that, the magnetic stirring apparatus in described step (1) and step (3) all adopts DF-101S instant-heating-type constant-temperature to heat magnetic stirring apparatus.
4. Regular Insulin according to claim 1 is applied to the method for coker gas oil desulfurization, it is characterized in that, described step (2) adopts water bath with thermostatic control magnetic stirring apparatus, and power is 40w.
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