CN101875870A - Method for preparing naphtha and diesel by blending waste oil - Google Patents
Method for preparing naphtha and diesel by blending waste oil Download PDFInfo
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- CN101875870A CN101875870A CN2009100834021A CN200910083402A CN101875870A CN 101875870 A CN101875870 A CN 101875870A CN 2009100834021 A CN2009100834021 A CN 2009100834021A CN 200910083402 A CN200910083402 A CN 200910083402A CN 101875870 A CN101875870 A CN 101875870A
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Abstract
The invention relates to a method for preparing naphtha and diesel by blending waste oil, which comprises the following main steps of: A) blending multiple kinds of waste oil to form blended stock, wherein the blended stock comprises 20 to 60 mass percent of chain hydrocarbon, 10 to 50 mass percent of cyclic hydrocarbon and 10 to 40 mass percent of aromatic hydrocarbon; B) mixing the blended stock and hydrogen and performing pre-hydrogenation reaction at the temperature of between 100 and 300 DEG C to remove impurities from the blended stock; and C) mixing the blended stock subjected to the pre-hydrogenation reaction in the step B and the hydrogen and performing hydrogenation reaction at the temperature of between 200 and 350 DEG C to obtain the naphtha and diesel.
Description
Technical field
The invention belongs to chemical industry and environmental protection field, in detail, relate to a kind of method of high-quality petroleum naphtha and fine-quality diesel oil fully of utilizing waste oil to be in harmonious proportion to produce next life.
Background technology
Because crude oil price skyrockets and impels the energetically exploitation of the world to new forms of energy and substitute energy, China is about the deep process technology exploitation and the industrial application Showed Very Brisk of coal tar since 2003.Only the patent application of coal tar hydrogenating is 21 more than, as coal tar hydrogenation process and catalyzer (number of patent application: 02122573.7), a kind of catalyst for coal tar hydrogenation modification and its production and application (number of patent application: 200510048573), a kind of technique for hydrogenation of coal oil (number of patent application: 200710012089), middle coal-tar heavy oil hydrocracking process (number of patent application 200410043708.1), a kind of coal tar hydro-conversion method and catalyzer (number of patent application 200410006256), coal tar hydrogenation modification reaction unit (number of patent application 200720031312), or the like.These patent common features are that the light component hydrogenation production cleaning component of tar and other waste oil reasonable compatibility methods are not all mentioned.
From the existing market situation, the comprehensive utilization of coal-tar pitch is the key of coal tar clean utilization.The enterprise of reconstructed coal tar has begun to pay attention to the clean utilization method of coal-tar pitch.Existing coal-tar pitch working method mainly is to produce the pitch blend component, produces water proof anti-corrosive paint, produces transformation of the way pitch, produces pitch coke, produces gac, is in harmonious proportion raw material etc. as needle coke.The coal-tar pitch lighting is that can coal tar produce cleaning product fully, reaches the key that environmental protection utilizes, and the lightweight oil that coal-tar pitch lighting such as coking produce still needs further desulfurization, denitrogenation, decarburization just can become environmental friendliness fuel.
Along with the nearly sustained and rapid development of economy of China, domestic waste oil kind is on the increase, except that coal tar, ethylene bottom oil, and waste oil that other output is bigger such as tire oil, plastics oil, shale oil, waste lubricating oil, swill oil or the like.Plastics oil, tire oil, the swill oil place of production disperse, and concentrated processing acquires a certain degree of difficulty.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing petroleum naphtha and diesel oil with the waste oil mediation, various waste oil are concentrated processing nearby, form reasonable compatibility according to raw material, the process hydrogenation technique is made with extra care and/or upgrading is produced clean diesel component and chemical industry light oil component afterwards.
For achieving the above object, provided by the inventionly be in harmonious proportion the method prepare petroleum naphtha and diesel oil with waste oil, its key step is:
A) various waste oil are reconciled into mixing raw material, in the mixing raw material after the mediation by mass percentage, chain hydrocarbon 20-60%, cyclic hydrocarbon 10-50%, aromatic hydrocarbons 10-40%;
B) mixing raw material mixes with hydrogen, carries out pre-hydrotreating reaction in 100-300 ℃, to remove the impurity in the mixing raw material;
C) step B is mixed with hydrogen through the mixing raw material of the anti-reaction of pre-hydrogenation, carry out hydrogenation reaction in 200-350 ℃, obtain petroleum naphtha and diesel oil.
In the steps A of the present invention,, can add proper amount of solvent it is dissolved each other fully if when various waste oil mutual solubility is relatively poor.The solvent that adopts is for having polar organic compound or mixture, as: a kind of or mixture in dodecylbenzene, methyl alcohol, ethanol, the washing oil.
The waste oil of indication of the present invention comprises: coal-tar heavy oil, middle coalite tar, ethylene bottom oil, converting plastic waste to oil, damaged tire oil, shale oil, waste lubricating oil, swill oil.
Among the step B of the present invention, pre-hydrotreating reaction is to carry out in the pre-hydrogenator of catalyst for pre-hydrogenation is housed, catalyst for pre-hydrogenation is diatomite, gac, natural plant fibre, potter's clay, kaolinic a kind of or several mixture arbitrarily, and it is reactive metal elemental nickel, molybdenum or the rhodium of 0-10% that catalyst for pre-hydrogenation also can load has mass percent.
Among the present invention, mixing raw material is 1 with the mixed volume ratio of hydrogen: 100-1: 150.
The present invention compared with prior art has following advantage:
The present invention is that important means solves that single waste oil ten alkane values are too low, material viscosity is crossed problems such as height with the feedstock optimization mediation.The present invention adopts pre-hydrogenation catalyst to remove the solid impurity of waste oil raw material, guarantees the hydrogenation unit long-term operation.Raw material variation of the present invention is carried out rational proportion to different material, and device adaptability improves, and region adaptability increases.The present invention pays attention to raw materials pretreatment, i.e. decarburization, deliming part etc.Catalyst for pre-hydrogenation of the present invention has strong adsorptive power, and pore structure distributes rationally, can recycle, and can not cause secondary pollution to environment.The mixing raw material cetane value that the present invention is in harmonious proportion can reach between the 30-55.
Description of drawings
Fig. 1 is a schematic flow sheet of the present invention.
Nomenclature in the accompanying drawing: 1-waste oil 1,2-waste oil 2,3-waste oil 3 or solvent, 4-mixing tank, 5-mixing waste oil, 6a, 6b-hydrogen, 7-pre-hydrogenator, the pre-hydrogenation waste oil of 8-, 9-hydrogenator, 10-hydrogenated products (diesel component and petroleum naphtha component mixture).
Embodiment
Cardinal principle of the present invention is described below:
The ultimate principle that with waste oil is raw material production fine-quality diesel oil component (comprising petroleum naphtha) is to adjust rational hydrocarbon system to form, chain hydrocarbon, cyclic hydrocarbon, aromatic hydrocarbons ratio near or equal the group composition of finished diesel fuel, the diesel component that hydrogenation and removing impurity production sulphur content, colourity, stability etc. are up to state standards, cetane value is between 30-55.Because of waste oil kind difference, its foreign matter content difference is as sulphur, nitrogen, heavy aromatics, uncombined carbon, ash the grade sulfur-nitrogen compound that can discharge atmosphere pollution after the burning, benzo pyrrole, carbon monoxide etc.Heavy aromatics, uncombined carbon and grey branch make carbonizing of engine and damage engine.Therefore the waste oil mixing raw material is adjusted after the qualified hydro carbons group composition, and combustionproperty is qualified, and its impurity must be removed.The method of hydrogenation can make sulfide become hydrogen sulfide stripping, and the nitride hydrogenation generates ammonia, saturated generation monocycle of heavy aromatics hydrogenation and double ring arene.In addition, different its smell differences in waste oil source because some organic compound has niff, even the very little smell of content is but very big in oil product, reach the purpose of taking off flavor thereby hydrogenation can destroy these materials that strange taste is arranged.
In a word, ultimate principle of the present invention is: form suitable raw material as diesel oil in order to obtain hydrocarbon system, different types of waste oil is in harmonious proportion.Raw material after being in harmonious proportion is adopted impurity such as method of hydrotreating desulfurization nitrogen, decolour, take off flavor, improve stability.
Key of the present invention is the material combination technology, waste oil raw material at different regions is in harmonious proportion, at first obtain hydrocarbon system and form the rational waste oil that mixes as hydrogenating materials, chain hydrocarbon content 20-60% (massfraction) in the mixing raw material, cyclic hydrocarbon content 10-50% (massfraction), aromaticity content 10-40% (massfraction), the raw material cetane value reaches about 45.When if various raw material mutual solubilities are relatively poor, can add proper amount of solvent it is dissolved each other fully.Exchange the raw material of becoming reconciled and carry out pre-treatment and take off uncombined carbon and the ash solid impurity that grades, guarantee the hydrogenator long-term operation, produce the fine-quality diesel oil component, finally realize the comprehensive clean utilization of multiple waste oil raw material, can not produce secondary pollution environment.
It can be direct mixing that raw material of the present invention is in harmonious proportion, and also can be to add the suitably mediation of other solvent.These solvents preferably have polar organic compound or mixture, as dodecylbenzene, methyl alcohol, ethanol, washing oil etc.
Catalyst for pre-hydrogenation of the present invention can be through the diatomite of adjusting pore structure and moulding, gac, natural plant fibre, potter's clay, kaolin etc. or their mixture.Its manufacture method is known hydrogenation catalyst manufacture method, grinds, operations such as moulding (add pore-forming template material), drying, saturated spray, calcining.Preferably use the gac or the vegetable fibre of large pore volume, and pre-hydrogenator preferably independently is set, the pre-hydrogenation agent after the use can be used as the raw material of wood-charcoal material and uses or material of construction.Also can be on the catalyst for pre-hydrogenation of the present invention according to trace active metal component in known preparation method's load, as metals such as nickel, molybdenum, rhodium, reactive metal component content 0-10% (massfraction).
According to above-mentioned basic ideas, the present invention has carried out a large amount of experimental studies, at first different waste oil is carried out chemical composition analysis, investigates wherein major impurity kind and content.Investigate various waste oil hydrocarbon system and form, study alkane wherein, cycloalkanes, aromaticity content and being in harmonious proportion ten alkane values, the condensation point of back product, the contribution of ignition characteristic.The chain hydrocarbon is maximum to the cetane value contribution in the fine-quality diesel oil, and cyclic hydrocarbon is bigger to reducing the contribution of condensation point and cold filter clogging temperature, and aromatic hydrocarbons can contribute big to flowability of diesel oil but cetane value is minimum.So the fine-quality diesel oil component is exactly the suitable mixture of collocation of three class hydrocarbon.
Sum up from different feedstock analysis data, coal tar, ethylene bottom oil are maximum with aromaticity content, be fit to produce high reformer feed of arene underwater content or benzene, naphthalene series products, another characteristics of coal tar are free carbon content height, coking value height (coking value of high temperature tar coal-tar pitch is up to 55).Plastics oil is in the majority with straight chain hydrocarbon, and waste lubricating oil is in the majority with naphthenic hydrocarbon, and swill oil, shale oil do not have outstanding feature in the hydro carbons group composition.Coal tar, ethylene bottom oil, plastics oil, shale oil are the thermo-cracking product, and common feature is uncombined carbon, ash oontent height.These solid impurity particle diameters are very little, and general filter method is difficult to remove.Because the existence of these fine particles, it is very fast that the pressure drop of coal tar hydrogenating reactor bed is risen, and there is hidden danger in long-term operation.Existing coal tar hydrogenating unit is a raw material with the coal tar light ends all, and the light ends of coal-tar heavy oil at all can't be separately as the hydrogenation charging, and its viscosity is big, uncombined carbon and ash oontent height blocking catalyst duct very easily, causes bed pressure drop to rise rapidly.
Below in conjunction with accompanying drawing technical process of the present invention is elaborated.
Different types of raw material 1,2,3 is that waste oil 1, waste oil 2, waste oil 3 or solvent at first carry out the physico-chemical property analysis among Fig. 1, calculate harmonic proportion according to hydro carbons group composition separately, enter mixing tank 4 according to calculating good ratio then, thorough mixing is even in mixing tank 4.The mixing waste oil 5 and the hydrogen 6a remix that mix are heated to suitable temperature (between 100-300 ℃) and enter pre-hydrogenator 7.Hydrogen and mixing waste oil by beds, carry out series of chemical and physical action at catalyst surface in pre-hydrogenator 7, the uncombined carbon in the mixing raw material 5, ash content, a small amount of sulphur nitrogen etc. are removed.The pre-hydrogenation waste oil 8 that comes out from pre-hydrogenator 7 mixes with another strand hydrogen 6b and is heated to and enters hydrogenator 9 between 200-350 ℃.Catalyzer in the hydrogenator 9 adopts industry to use sophisticated hydrofining or hydrotreating catalyst.Hydrogenated oil 10 through impurity such as hydrogenator 9 deep desulfuration nitrogen obtains petroleum naphtha and fine-quality diesel oil component through after the fractionation.
Embodiment one
Pre-hydrogenation main technologic parameters sees Table 2.The catalyst for pre-hydrogenation main character sees Table 3.Product main character after the fractionation sees Table 4.
Table 1 waste oil raw material main character
| | Waste oil | 1 | |
|
| Density (20 ℃), g/m 3 | ??1.01 | ??0.91 | ??0.95 | |
| Elementary composition, μ g/g | ||||
| Sulphur | ??5000 | ??100 | ??20000 | |
| Nitrogen | ??6000 | ??80 | ??150 | |
| Condensation point, ℃ | ??70 | ??35 | ??40 | |
| Uncombined carbon, m% | ??15 | ??10 | ??17 | |
| Ash content, m% | ??2 | ??1 | ??2.5 | |
| Cetane value | ??29 | ??48 | ??38 | |
| Hydrocarbon system forms, m% | ||||
| Paraffinic hydrocarbons | ??0 | ??60 | ??45 | |
| Naphthenic hydrocarbon | ??10 | ??0 | ??10 | |
| Aromatic hydrocarbons | ??60 | ??20 | ??20 | |
| Colloid etc. | ??30 | ??20 | ??25 | |
| The cut scope, ℃ | ??90-360 | Fore-running-400 | Fore-running-400 |
The pre-hydroprocessing condition of table 2
| Title | |
| Pressure, MPa (gauge pressure) | ??6.0 |
| Title | |
| Temperature, ℃ | ??240 |
| Air speed, h -1 | ??0.8 |
| Hydrogen-oil ratio (volume ratio) | ??150∶1 |
Table 3 catalyzer main character
| Title | |
| Carrier, m% | 100% Pericarppium arachidis hypogaeae gac |
| Active constituent, m% | ??0 |
| Pore volume, m 2/g | ??900 |
| Shape, mm | Hollow posts, 200 * 10-50 |
Table 4 hydrogenated products main character (product after the fractionation)
| Title | Hydrotreated naphtha | The hydrogenated diesel oil component |
| Density (20 ℃), g/m 3 | ??0.80 | ??0.89 |
| Elementary composition, μ g/g | ||
| Sulphur | ??50 | ??50 |
| Nitrogen | ??10 | ??200 |
| Condensation point, ℃ | ??/ | ??0 |
| Cetane index (ASTM D4737) | ??/ | ??41 |
| Boiling range (ASTM D86), ℃ | ||
| Initial boiling point | ??70 | ??170 |
| ??10％ | ??90 | ??200 |
| ??50％ | ??120 | ??240 |
| Title | Hydrotreated naphtha | The hydrogenated diesel oil component |
| ??90％ | ??150 | ??340 |
| Final boiling point | ??190 | ??385 |
Embodiment two
Pre-hydrogenation main technologic parameters sees Table 6.The catalyst for pre-hydrogenation main character sees Table 7.Product main character after the fractionation sees Table 8.
Table 5 waste oil raw material main character
| | Waste oil | 1 | |
|
| Density (20 ℃), g/m 3 | ??0.988 | ??0.87 | ??0.88 | |
| Elementary composition, μ g/g | ||||
| Sulphur | ??5000 | ??1000 | ??650 | |
| Nitrogen | ??7000 | ??2000 | ??550 | |
| Condensation point, ℃ | ??60 | ??0 | ??10 | |
| Uncombined carbon, m% | ??12 | ??5 | ??11 | |
| Ash content, m% | ??1.5 | ??0.6 | ??5 | |
| Cetane value | ??32 | ??40 | ??43 | |
| Hydrocarbon system forms, m% | ||||
| Paraffinic hydrocarbons | ??18 | ??40 | ??20 | |
| Naphthenic hydrocarbon | ??20 | ??15 | ??55 |
| | Waste oil | 1 | |
|
| Aromatic hydrocarbons | ??42 | ??30 | ??10 | |
| Colloid etc. | ??20 | ??15 | ??15 | |
| The cut scope, ℃ | Fore-running-380 | Fore-running-380 | Fore-running-380 |
The pre-hydroprocessing condition of table 6
| Title | |
| Pressure, MPa (gauge pressure) | ??8.0 |
| Temperature, ℃ | ??320 |
| Air speed, h -1 | ??0.8 |
| Hydrogen-oil ratio (volume ratio) | ??150∶1 |
Table 7 catalyzer main character
| Title | |
| Carrier, m% | Macropore porcelain ball |
| Active constituent, m% | 1% nickel |
| Pore volume, m 2/g | ??700 |
| Shape, mm | ??ф3-25 |
Table 8 hydrogenated products main character (product after the fractionation)
| Title | Hydrotreated naphtha | The hydrogenated diesel oil component |
| Density (20 ℃), g/m 3 | ??0.78 | ??0.87 |
| Elementary composition, μ g/g | ||
| Sulphur | ??50 | ??50 |
| Title | Hydrotreated naphtha | The hydrogenated diesel oil component |
| Nitrogen | ??100 | ??400 |
| Condensation point, ℃ | ??/ | ??0 |
| Cetane index (ASTM D4737) | ??/ | ??40 |
Claims (9)
1. one kind is in harmonious proportion the method prepare petroleum naphtha and diesel oil with waste oil, and its key step is:
A) various waste oil are reconciled into mixing raw material, in the mixing raw material after the mediation by mass percentage, chain hydrocarbon 20-60%, cyclic hydrocarbon 10-50%, aromatic hydrocarbons 10-40%;
B) mixing raw material mixes with hydrogen, carries out pre-hydrotreating reaction in 100-300 ℃, to remove the impurity in the mixing raw material;
C) step B is mixed with hydrogen through the mixing raw material of the anti-reaction of pre-hydrogenation, carry out hydrogenation reaction in 200-350 ℃, obtain petroleum naphtha and diesel oil.
2. method according to claim 1 wherein, when steps A is mixed various waste oil, adds solvent and is in harmonious proportion.
3. method according to claim 2, wherein, solvent is for having polar organic compound or mixture.
4. method according to claim 3, wherein, solvent is a kind of or mixture in dodecylbenzene, methyl alcohol, ethanol, the washing oil.
5. method according to claim 1 and 2, wherein, waste oil comprises: coal-tar heavy oil, middle coalite tar, ethylene bottom oil, converting plastic waste to oil, damaged tire oil, shale oil, waste lubricating oil, swill oil.
6. method according to claim 1, wherein, the pre-hydrotreating reaction of step B is to carry out in the pre-hydrogenator of catalyst for pre-hydrogenation is housed.
7. method according to claim 6, wherein, catalyst for pre-hydrogenation is diatomite, gac, natural plant fibre, potter's clay, kaolinic a kind of or any several mixture.
8. method according to claim 7, wherein, it is reactive metal elemental nickel, molybdenum or the rhodium of 0-10% that pre-hydrogenation agent catalyst cupport has mass percent.
9. method according to claim 1, wherein, mixing raw material is 1 with the mixed volume ratio of hydrogen: 100-1: 150.
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| CN102304392A (en) * | 2011-08-04 | 2012-01-04 | 孔永平 | Composite biodiesel and preparation method thereof |
| CN106554828A (en) * | 2015-09-24 | 2017-04-05 | 中国石油化工股份有限公司 | A kind of heavy fuel fluid composition and preparation method thereof |
| CN109575988A (en) * | 2017-09-28 | 2019-04-05 | 中国石油化工股份有限公司 | The method of tar made fuel oil |
| CN109651850A (en) * | 2019-02-18 | 2019-04-19 | 山西永东化工股份有限公司 | A kind of coal tar carbolineum desulfurization deliming and production superconductive carbon black method |
| CN109694653A (en) * | 2017-10-23 | 2019-04-30 | 湖南长岭石化科技开发有限公司 | The production method of highly hydrogenated rosin |
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2009
- 2009-04-29 CN CN2009100834021A patent/CN101875870A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304392A (en) * | 2011-08-04 | 2012-01-04 | 孔永平 | Composite biodiesel and preparation method thereof |
| CN106554828A (en) * | 2015-09-24 | 2017-04-05 | 中国石油化工股份有限公司 | A kind of heavy fuel fluid composition and preparation method thereof |
| CN106554828B (en) * | 2015-09-24 | 2021-03-05 | 中国石油化工股份有限公司 | Heavy fuel oil composition and preparation method thereof |
| CN109575988A (en) * | 2017-09-28 | 2019-04-05 | 中国石油化工股份有限公司 | The method of tar made fuel oil |
| CN109575988B (en) * | 2017-09-28 | 2020-12-29 | 中国石油化工股份有限公司 | Method for preparing fuel oil from tar |
| CN109694653A (en) * | 2017-10-23 | 2019-04-30 | 湖南长岭石化科技开发有限公司 | The production method of highly hydrogenated rosin |
| CN109651850A (en) * | 2019-02-18 | 2019-04-19 | 山西永东化工股份有限公司 | A kind of coal tar carbolineum desulfurization deliming and production superconductive carbon black method |
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Application publication date: 20101103 |