CN102226104A - Method for producing gasoline and diesel by utilizing waste lubricating oil - Google Patents
Method for producing gasoline and diesel by utilizing waste lubricating oil Download PDFInfo
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- CN102226104A CN102226104A CN2011101341067A CN201110134106A CN102226104A CN 102226104 A CN102226104 A CN 102226104A CN 2011101341067 A CN2011101341067 A CN 2011101341067A CN 201110134106 A CN201110134106 A CN 201110134106A CN 102226104 A CN102226104 A CN 102226104A
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Abstract
The invention discloses a method for producing gasoline and diesel by utilizing waste lubricating oil, belonging to the technical field of environmental protection and energy. The method is characterized in that the lubricating oil is used as the raw material and is subjected to reactive distillation, hydrofining and distillation to produce the high-quality gasoline and diesel; firstly the waste lubricating oil is subjected to reactive distillation to adjust the proportion of gasoline and diesel and reduce the content of colloid; then hydrofining reaction is carried out on a sulfide catalyst; monoene compounds are removed through monoolefine hydrogenation saturation reaction; sulfur, nitrogen and colloid are removed to produce the high-quality gasoline and diesel mixture free from extraneous odour; and the gasoline and diesel mixture is distilled to obtain gasoline and diesel distillates; wherein the sulfide catalyst is prepared by selecting an appropriate carrier according to the composition and properties of the pyrolysis plastic oil and adopting a liquid phase method. The method has the advantages of simple process, high catalyst activity and selectivity and good economic benefits and industrial application prospect.
Description
Technical field
The invention belongs to environment protection and energy technology field, relate to a kind of method of utilizing waste lubricating oil to produce petrol and diesel oil.
Background technology
The waste lubricating oil of Chinese market comes from two parts in motor vehicle market and industrial production field.According to analysis to motor vehicle market and waste lubricating oil market growth, industrial production field speed, follow the quick growth of Chinese motor vehicle market recoverable amount, the time coming years, the waste lubricating oil market growth speed in Chinese motor vehicle market will keep very fast level.By contrast, owing to be subjected to the influence of aspect policy such as state macro-control, waste lubricating oil market growth, industrial production field speed will keep stable growth.After 2006, Chinese motor vehicle market waste lubricating oil market capacity will be above industrial production field waste lubricating oil market capacity.According to the just slightly investigation at an ancient unit of weight plan Management Advisory Services industry research center, Chinese waste lubricating oil market capacity was 5,000,000 tons in 2010, the production of China's lube product and use belong to the line style economic model of traditional industrial society's one-way type flow of resources, i.e. " petroleum resources one refining lube product one waste lubricating oil is abandoned " pattern.The waste oil regeneration rate is compared with developed country bigger gap.In general, can should be about 50% of consumption for the lubricants capacity that reclaims, yet the recovery utilization rate of waste lubricating oil is very low at present, the rerefined oil that returns usefulness every year is less than 10%, a considerable amount of waste lubricating oils flow to not clear, and wherein a part enters environment and pollutes.Outside contamination produces a large amount of colloids, oxide compound reduces and even lost due effect meets with discarded thereby lubricating oil is owing in use being subjected to.State Bureau of Environmental Protection has been classified waste lubricating oil as this century at one of three big emphasis of environmental protection field major control, and make full use of waste lubricant oil regeneration reduction finished lube, or waste lubricating oil is refined into gasoline, diesel oil, can alleviate the China's oil shortage and the growing imbalance between supply and demand of demand, can promote environmental protection again, turn waste into wealth, create considerable economic, be the project that country encourages support, prospect is very wide.
At abundant waste lubricating oil recycling problem, according to the chemical constitution and the character of waste lubricating oil, we have successfully developed the new technology that petrol and diesel oil is produced in waste lubricating oil catalytic distillation-hydrogenation upgrading-air distillation.The useless lubricated catalyzer that adopts with intellecture property, the cut ratio by catalytic distillation transformation technology adjustment petrol and diesel oil reduces the gum level in the cut; Carry out hydrofining again and obtain distillate, distillate is produced the high-quality petrol and diesel oil of market in urgent need etc. through the normal pressure distillation.The no three wastes produce in air distillation or catalytic distillation-hydrogenation upgrading-air distillation, are a processes green, recycling.Following known technology all comes with some shortcomings:
Chinese patent, publication number: CN201010182957.4, the method and the device thereof of introduction Separation and Recovery processed oil from waste lubricating oil, its operation is more, and is more loaded down with trivial details, produce " three wastes ", and product quality is low.
Chinese patent, publication number: CN201010160808.8 introduces the method for utilizing waste oil processing liquid fuel oil, and its operation is many, and waste liquid is many, and the product quality that obtains is low.
Chinese patent, publication number: CN201010151513.4 introduces a kind of preparation method of reclaimed lubricating oil fraction, and its process will be used sorbent material, and it is higher to consume a large amount of sorbent material expenses, and the oil quality that obtains is low.
Chinese patent, publication number: CN201010132513.X introduces a kind of used lubricating oil complete hydrogenation type regenerated catalyst and its production and application, and it crosses range request 15MPa high pressure, high hydrogen-oil ratio, consumption hydrogen is many, and the product performance that obtain are poor.
Chinese patent, publication number: CN200920141806.7, the novel appts of introduction refining light diesel from waste lubricating oil, the diesel quality that obtains is low, and product yield is low.
Summary of the invention
The invention provides that a kind of method of utilizing waste lubricating oil to produce petrol and diesel oil is low at the product specification in the waste lubricating oil conversion process, deficiency in economic performance and secondary pollution problems, with the petrol and diesel oil is that target product realizes that waste lubricating oil carries out recycling, and the waste residue and the combustion gas of comprehensive utilization process itself, make the energy-conservation and environmental protection of production process, avoided secondary pollution.Through catalytic reaction distillation, air distillation is passed through in the hydrogenation upgrading again with waste lubricating oil in the present invention, cuts into gasoline (<150 ℃) and diesel oil (>150 ℃) according to recovered temperature.The present invention improved the transformation efficiency of balanced reaction and consecutive reaction selectivity, energy-conservation of consumption reduction, prolonged catalyst life, flow process is simple and reduce investment outlay.
Technical scheme of the present invention is as follows:
Waste lubricating oil raw material waste lubricating oil among the present invention comprises gasoline, bavin machine oil, shafting oil, hydraulic efficiency oil, wear-resistant pressure oil, transformer oil, various lubricating grease and washes part oil, be one or two or more kinds mixing wherein, also can select the waste rubber of rubber item as raw material.
The catalyzer that uses among the present invention is the molecular sieve of alumina load, and wherein molecular sieve comprises ZSM-5, y-type zeolite, mordenite and β zeolite or their mixture, and molecular sieve content is 0.5-95wt%.The size of preformed catalyst determines that according to the diameter of reaction fractionating tower the equivalent diameter of general granules of catalyst should be less than 0.1 with the diameter ratio of reaction fractionating tower.The main effect of catalyzer is the selective splitting macromole, and carries out isomerization reaction simultaneously and obtain corresponding petrol and diesel oil cut.Catalyzer also is the filler of rectifying tower in addition, is used for reacting separating of product and product cut.
This method is that waste lubricating oil is carried out in reaction fractionating tower at gas phase catalysis cracking process on molecular sieve/aluminium oxide catalyst and the process integration of reactor product fractionation separates.The raw material waste lubricating oil is injected still kettle, adopt the waste residue and the combustion gas that produce in the waste lubricating oil conversion process to heat, the still kettle temperature is controlled between 250-500 ℃.When the still kettle heating arrived 250 ℃, the oil gas that distills entered in the reaction fractionating tower that molecular sieve/aluminium oxide catalyst is housed and reacts and rectifying, and agent-oil ratio is controlled between the 1-20.Waste lubricating oil enters with hydrogen by feedstock pump through the cut of catalytic distillation and mixes after the interchanger heating enters hydrofining reactor, and the control feeding temperature is at 250-350 ℃; Hydrogen partial pressure 1-6MPa, volume space velocity 0.5-4.0h-1 and hydrogen to oil volume ratio are 100-1000: 1; The sulfide catalyst that hydrogenation uses is loading type NiMo, NiW, CoMo, CoW, NiMoW or CoMoW sulfide catalyst, and carrier is oxide carrier or the raw material of wood-charcoal material with two mesopore composite structures, and oxide carrier is SiO
2, Al
2O
3, TiO
2, SiO
2-Al
2O
3Or Al
2O
3-TiO
2Distillate after the hydrofining distills through normal pressure, cuts into gasoline (<150 ℃) and diesel oil (>150 ℃) according to recovered temperature.
By method production of the present invention obtain gasoline fraction (<150 ℃〉yield at 20-30%, octane value is 75-85, density 0.70-0.76g/cm
3, can be used as the blend component of gasoline.The yield of diesel oil distillate (150-360 ℃) is at 60-80%, and cetane value is 65, density 0.83-0.86g/cm
3, condensation point is lower than-20 ℃, can be used as low-coagulation diesel oil No. 10.Combustion gas and cinder productive rate are not higher than 8%.
The mode of operate continuously, flexible operation, easy are adopted in catalytic distillation of the present invention, hydrofining and air distillation.
The present invention adopts air distillation to combine with the gas phase catalysis cracking process, and the combustion gas and the cinder that make full use of process have reduced energy consumption, non-secondary pollution; Improve the transformation efficiency of balanced reaction by air distillation and catalytic rectification process, improved the selectivity of reaction, prolonged the Hydrobon catalyst life-span, reduced catalyst levels simultaneously; Elder generation's fractionation repeated hydrogenation has reduced the hydrogen consumption; Product yield height, wide scope of material.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Among the figure: 1 heating kettle; 2 reactive distillation columns, 3 hydrofining reaction towers; 4 distillation towers.
Embodiment
Be described in detail specific embodiments of the invention below in conjunction with technical scheme and accompanying drawing.
Embodiment 1: the gas phase catalysis cracking of waste lubricating oil on molecular sieve/aluminium oxide catalyst.Heavy oil is injected the reaction fractionating tower that molecular sieve/aluminium oxide catalyst is housed to react and the rectifying distillation tower, catalyzer is made up of the aluminum oxide that contains 30%ZSM-5 and 10% β zeolite, obtain the columnar product of 2.0-3.0mm by molding bonded, length 3-8mm, bulk density 0.65-0.80g/mL, intensity is greater than 40N/mm.Adopt the waste residue and the combustion gas that produce in the converting plastic waste to oil conversion process to heat, agent-oil ratio is controlled between the 1-20.The combustion gas that produces is used for the heating of distillation tower.Following table 1 is seen catalytic distillation material balance test-results
Following table 2 is seen catalytic distillation front and back oil property
Raw material | Waste lubricating oil | Catalytic distillation |
Density/gcm -1 | 0.88 | 0.81 |
Sulphur/ppm | 9300 | 2200 |
Nitrogen/ppm | 2800 | 2200 |
Acid number/mgKOH.g -1 | 3.6 | 3.2 |
Color | Chocolate | Sorrel |
Have or not stink | Have | Have |
Embodiment 2: supported cobalt molybdenum sulphide catalyzer is a Hydrobon catalyst.Carrier adopts SiO
2-Al
2O
3, specific surface area is at 200-400m
2/ g, pore volume is at 0.5-2.0cm
3/ g, the most probable pore size distribution is at 2-4nm and 10-15nm.Cobalt molybdenum sulphide precursor adopts Xiao Suangu or Cobaltous diacetate or acetylacetone cobalt and ammonium thiomolybdate.Adopt equi-volume impregnating to prepare supported cobalt molybdenum sulphide catalyzer through dipping-drying-steps such as roasting.Following table 3 is seen reaction process condition and product composition.
Phase run | Initial stage/latter stage |
Reactor hydrogen dividing potential drop/MPa | 4 |
Volume space velocity/h -1 | 0.5 |
The reactor inlet hydrogen to oil volume ratio | 800 |
Average reaction temperature/℃ | 300 |
Product property | |
Diene/g. (100g) -1 | 0 |
Colloid/mg100mL -1 | 25 |
Nitrogen/μ gg -1 | 3 |
Sulphur/μ gg -1 | 46 |
Other | The color water-white |
As shown in Table 3, oil distillate on supported cobalt molybdenum sulphide catalyzer in 300 ℃ of hydrofinings, do not detect diolefine in the product that obtains, the content of colloid, sulphur and nitrogen reduces greatly, shows that supported cobalt molybdenum sulphide catalyzer has good desulfurization removing nitric deolefination efficient.The product water-white that obtains, free from extraneous odour, the petrol and diesel oil mixture that quality is high.
Embodiment 3: the product after the hydrofining enters atmospheric distillation tower and cuts into gasoline (<150 ℃) and diesel oil (>150 ℃) according to recovered temperature.4 tables are seen vapour, diesel oil character down
Gasoline | Diesel oil | |
Density/gcm -1 | 0.72 | 0.82 |
Diene/g. (100g) -1 | 0 | 0 |
Colloid/mg100mL -1 | 2 | 20 |
Nitrogen/μ gg -1 | 8 | 3 |
Sulphur/μ gg -1 | 90 | 40 |
Other | Color: water-white; Octane value: 75 | Color: pale yellow; Cetane value: 65 |
As shown in Table 4, oil distillate obtains the petrol and diesel oil distillate through atmospheric distillation.The product free from extraneous odour that obtains, gasoline that quality is high and diesel oil.
Embodiment 3: the catalytic distillation distillate is a raw material, carries out stability experiment 4.0MPa and 300 ℃ on the basis of embodiment 1,2,3, and following table 5 is seen the reaction process condition of operation in 200 hours and obtained product property at last.
Gasoline | Diesel oil | |
Diene/g. (100g) -1 | 0 | 0 |
Colloid/mg100mL -1 | 2 | 21 |
Nitrogen/μ gg -1 | 8 | 3 |
Sulphur/μ gg -1 | 90 | 40 |
Other | Color: water-white; Octane value: 75 | Color: pale yellow; Cetane value: 65 |
200 hours experimental result in 300 ℃ of hydrofinings, does not detect diolefine in the petrol and diesel oil product that air distillation obtains on load-type nickel molybdenum sulphide catalyzer as shown in Table 4, reaches 2mg100mL for gasoline gum content
-1, also be reduced to 21mg100mL for the diesel oil gum level
-1, containing with beginning test of sulphur and nitrogen compared constantly substantially, meets national petrol and diesel oil standard, shows the product free from extraneous odour that this technology obtains, and has good stability the vapour that quality is high, diesel oil.The above results shows that technology of the present invention has satisfactory stability.
Claims (8)
1. method of utilizing waste lubricating oil to produce petrol and diesel oil, waste lubricating oil carries out in reaction fractionating tower at gas phase catalysis cracking process on molecular sieve/aluminium oxide catalyst and the process integration of reactor product fractionation separates; It is characterized in that: waste lubricating oil is injected still kettle, adopt the waste residue and the combustion gas that produce in the waste lubricating oil conversion process to heat, the still kettle temperature is controlled at 250-500 ℃; The oil gas that distills enters in the reaction fractionating tower that molecular sieve/aluminium oxide catalyst is housed and reacts and rectifying, and agent-oil ratio is controlled at 1-20; Waste lubricating oil enters hydrofining reaction tower, feeding temperature 250-350 ℃, hydrogen partial pressure 1-6MPa, volume space velocity 0.5-4.0h through the interchanger heating behind the catalytic pyrolysis
-1, hydrogen to oil volume ratio 100-1000: 1; The sulfide catalyst that hydrogenation uses is the loading type sulfide catalyst; Carrier is the oxide carrier with two mesopore composite structures; Distillate after the hydrofining distills through normal pressure, cuts into gasoline and diesel oil according to recovered temperature.
2. a kind of method of utilizing waste lubricating oil to produce petrol and diesel oil according to claim 1, its feature also is: described sulfide catalyst is NiMo, NiW, CoMo, CoW, NiMoW or CoMoW.
3. a kind of method of utilizing waste lubricating oil to produce petrol and diesel oil according to claim 1, its feature also is: described oxide carrier with two mesopore composite structures is SiO
2, Al
2O
3, TiO
2, SiO
2-Al
2O
3Or Al
2O
3-TiO
2
4. according to claim 1,2 or 3 described methods, its feature also is: waste lubricating oil comprises gasoline, bavin machine oil, shafting oil, hydraulic efficiency oil, wear-resistant pressure oil, transformer oil, various lubricating grease and washes part oil, is one or two or more kinds mixing wherein.
5. according to claim 1,2 or 3 described methods, its feature also is: reaction distillation, hydrofining and distillation operate continuously.
6. method according to claim 4, its feature also is: reaction distillation, hydrofining and distillation operate continuously.
7. according to claim 1,2 or 3 described methods, its feature also is: waste rubber oil replaces waste lubricating oil as raw material.
8. a kind of method of utilizing waste lubricating oil to produce petrol and diesel oil according to claim 4, its feature also is: waste rubber oil replaces waste lubricating oil as raw material.
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Cited By (7)
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CN102676219A (en) * | 2012-05-15 | 2012-09-19 | 大连理工大学 | Method for utilizing coal tar to produce gasoline and diesel |
CN102786985A (en) * | 2012-07-27 | 2012-11-21 | 大连理工大学 | Resource utilization method for waste lubricating oil |
CN103484156A (en) * | 2013-08-29 | 2014-01-01 | 连力生 | Method for producing diesel through spent lubrication oil and production device thereof |
CN103555367A (en) * | 2013-11-25 | 2014-02-05 | 辽宁中旭石油化工有限公司 | Method for producing naphtha, diesel oil and lubricant base oil by using used lubrication oil |
CN104399512A (en) * | 2014-12-10 | 2015-03-11 | 郭帅 | Novel efficient and environment-friendly catalyst for waste tire oil regeneration |
CN104650949A (en) * | 2013-11-20 | 2015-05-27 | 东营争峰新能源技术有限公司 | Device for producing diesel oil through catalytic distillation of waste engine oil |
CN112717946A (en) * | 2020-12-31 | 2021-04-30 | 西北化工研究院有限公司 | Spent lubricating oil hydrogenation regeneration catalyst and preparation method thereof |
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CN101475870A (en) * | 2009-01-17 | 2009-07-08 | 大连理工大学 | Method for producing petrol and diesel oil by recycling waste lubricant oil |
CN101845323A (en) * | 2010-05-14 | 2010-09-29 | 大连理工大学 | Process for producing petrol and diesel oil by plastic oil |
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102676219A (en) * | 2012-05-15 | 2012-09-19 | 大连理工大学 | Method for utilizing coal tar to produce gasoline and diesel |
CN102786985A (en) * | 2012-07-27 | 2012-11-21 | 大连理工大学 | Resource utilization method for waste lubricating oil |
CN102786985B (en) * | 2012-07-27 | 2015-01-07 | 大连理工大学 | Resource utilization method for waste lubricating oil |
CN103484156A (en) * | 2013-08-29 | 2014-01-01 | 连力生 | Method for producing diesel through spent lubrication oil and production device thereof |
CN103484156B (en) * | 2013-08-29 | 2016-03-02 | 连力生 | A kind of waste lubricating oil produces method and the production equipment thereof of diesel oil |
CN104650949A (en) * | 2013-11-20 | 2015-05-27 | 东营争峰新能源技术有限公司 | Device for producing diesel oil through catalytic distillation of waste engine oil |
CN103555367A (en) * | 2013-11-25 | 2014-02-05 | 辽宁中旭石油化工有限公司 | Method for producing naphtha, diesel oil and lubricant base oil by using used lubrication oil |
CN104399512A (en) * | 2014-12-10 | 2015-03-11 | 郭帅 | Novel efficient and environment-friendly catalyst for waste tire oil regeneration |
CN104399512B (en) * | 2014-12-10 | 2017-01-11 | 郭帅 | Efficient and environment-friendly catalyst for waste tire oil regeneration |
CN112717946A (en) * | 2020-12-31 | 2021-04-30 | 西北化工研究院有限公司 | Spent lubricating oil hydrogenation regeneration catalyst and preparation method thereof |
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