CN103484156B - A kind of waste lubricating oil produces method and the production equipment thereof of diesel oil - Google Patents
A kind of waste lubricating oil produces method and the production equipment thereof of diesel oil Download PDFInfo
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Abstract
The invention discloses the method that waste lubricating oil produces diesel oil, waste lubricating oil and catalyzer are heated to 180-410 DEG C of reaction, be gas oil by the oil phase that the cut condensation produced at this temperature obtains, be diesel product after gas oil is refining, the catalyzer used is by 1-10wt% ferric oxide, 1-10wt% magnesium oxide, 20-40wt% γ-Al
2o
3and/or η-Al
2o
3, 3-20wt% calcium oxide and 20-40wt% silicon-dioxide composition.The present invention also proposes the method production equipment, comprise reactor, burner, condenser, oil-gas separator, air water separator, temperature sensor, liquid level sensor, gas phase catalysis device, head tank, preheater and fuel oil drum, fuel is lighted a fire in the combustion chamber of burner, flue gas is except for except reacting by heating still, in flue, also enter in preheater the oil plant heating and dewatered successively, the evaporant of reactor is sent into further or directly sends into condensation in condenser after gas phase catalyst catalysis, condensation product is through oil-gas separator, refine after air water separator process and obtain diesel oil, its diesel yield reaches more than 85%.
Description
Technical field
The present invention relates to a kind of method that waste lubricating oil produces diesel oil, and use the production equipment of the method, belong to waste oil treatment technical field.
Background technology
The machinery of most type all will use lubricating oil, and this is because lubricating oil can reduce frictional force between machinery or between parts, to protect the surface of machinery or parts, to reduce wear, and the work-ing life of prolonged mechanical.Lubricating oil is the doping of petroleum refining base oil and refines to obtain, and its output accounts for about 2% of petroleum products total amount.Because the environment for use of dissimilar machinery differs greatly, therefore lubricating oil easily goes bad because of generation physics or chemical transformation and becomes waste lubricating oil in various complex environment.
For the process of waste lubricating oil, at present mostly both at home and abroad to use after waste lubricant oil regeneration, its process is: waste lubricating oil is after sedimentation, filtration, absorption remove most of impurity, its water content is reduced again through dehydration, then the waste lubricant oil by hydrogenation processed is refined to remove the materials such as oxide compound, sulfocompound, halogen compounds, nitride and the heavy metal compound in waste oil, obtain spendable rerefined oil finally by after blending.But above-mentioned reclaiming process thoroughly cannot remove the impurity of waste lubricating oil, rerefined oil is still containing some impurity, and the existence of these impurity reduces the quality of rerefined oil; Further, process for regeneration of waste lubricating oil is complicated, energy consumption is very high, easily to environment; In addition, the oil product finally obtained could use as rerefined oil after needing additionally to add the blending of other materials, and this makes process for regeneration of waste lubricating oil more complicated, and cost is higher, is unfavorable for promoting the use of.
Because process for regeneration of waste lubricating oil has above-mentioned technical problem, and those skilled in the art can not find better solution for the problems referred to above always, therefore present research turns, pay close attention to approach waste lubricating oil lightweight being turned to fuel and directly use more, as Chinese patent literature CN101029247A discloses a kind of method that waste lubricating oil produces diesel oil, waste lubricating oil first loads in still kettle and adds thermal distillation by it, in still kettle, add the mordenite of waste lubricating oil weight 0.5-2% as catalyzer simultaneously, distillation temperature controls to complete fore-running at 125-380 DEG C, the distillate obtained puts into stirrer again, and the industrial sulphuric acid adding distillate weight 1-1.5% stirs 2-3 hour, then 3-5 hour is left standstill, getting supernatant liquor adds in stirrer, the industrial sulphuric acid adding supernatant liquor weight 1-1.5% again carries out stirring 2-3 and as a child left standstill 3-5 hour, getting supernatant liquor afterwards again adds in stirrer, add the sodium hydroxide of supernatant liquor weight 1-1.5%, the concentration of sodium hydroxide is 25-30%, stir after 2-3 hour, then leave standstill 3-5 hour, the supernatant liquor obtained is diesel oil.
Above-mentioned waste lubricating oil diesel oil technique directly can obtain diesel oil fuel, and technique is simple, be easy to promote.But, above-mentioned technique carrying out adding acid for many times to distillate, add in alkali process and can produce a large amount of acid-base waste fluid, these liquid waste disposal are improper easily to environment; And above-mentioned technique needs the plenty of time to stir and standing liquid, and process cycle is long, production efficiency is low; In addition, above-mentioned technique need repeatedly get supernatant liquor to distillate and the process of process, and the supernatant liquor finally obtained is only diesel product, and thus the diesel yield of above-mentioned technique is lower, and the randomness of getting supernatant liquor operation is very large, is easy to the quality affecting diesel product.
Summary of the invention
The present invention relates to a kind of method that waste lubricating oil produces diesel oil, and use the production equipment of the method, belong to waste oil treatment technical field.
Summary of the invention
Technical problem to be solved by this invention can produce a large amount of waste liquid when processing distillate in prior art, the easy contaminate environment of waste liquid, and the process cycle of prior art is long, efficiency is low; And then a kind of method of environmental protection, the diesel oil of waste lubricating oil production is efficiently proposed.
Another technical problem to be solved by this invention be in prior art to distillate repeatedly get supernatant liquor and process after, the supernatant liquor finally obtained is only diesel product, and diesel yield is lower; And then the waste lubricating oil proposing a kind of high yield produces the method for diesel oil.
For solving the problems of the technologies described above, the invention provides a kind of method that waste lubricating oil produces diesel oil, comprising the steps,
(1) in waste lubricating oil, add catalyzer, heat and remain on 180-410 DEG C, the cut steamed under obtaining said temperature;
(2) the oil phase thing described cut condensation obtained is refined;
Described catalyzer is made up of the component of following weight percent: ferric oxide 1-10%, magnesium oxide 1-10%, γ-Al
2o
3and/or η-Al
2o
320-40%, calcium oxide 3-20%, silicon-dioxide 20-40%.
The temperature rise rate starting to heat is 0.3-3 DEG C/min.
The temperature of described heating is 340-370 DEG C.
Described catalyst weight is the 0.05-5% of described useless lubrication weight.
First described cut fraction section condensation is obtained mink cell focus phases and gas gas-phase objects, then the two sections of condensations of described gas gas-phase objects are obtained lightweight oil phases; Obtain heavy diesel by refining for described mink cell focus phases, obtain LIGHT DIESEL OIL by refining for described lightweight oil phases.
On this basis, also propose the production equipment of aforesaid method, comprise
Reactor, is provided with oil-in, and top or top are provided with vapour outlet;
Heating installation, comprises interconnective function unit and heat release parts, and at least part of described heat release parts are arranged in described reactor or described heat release components interior is connected with described reactor inside;
Condenser, is provided with import and outlet, and the import of described condenser is connected with the vapour outlet of described reactor;
Oil-gas separator, is provided with import, air outlet and oil outlet, and the import of described oil-gas separator is connected with the outlet of described condenser;
Air water separator, comprises import and water outlet, and the import of described air water separator is connected with the air outlet of described oil-gas separator;
For measuring the thermoscope of described reactor temperature, the temperature-sensitive position of described thermoscope is arranged in described reactor.
In described heating installation, described function unit is burner, and described heat release parts are the combustion chamber being positioned at described reactor; Described production equipment also comprises chimney, and the import of described chimney is connected with the outlet of described combustion chamber through reactor wall, and the exit of described chimney is provided with smoke purifier.
Also comprise the head tank, flue and the preheater that are provided with outlet; Described preheater comprises urceolus and is arranged at the oil feed passage in described urceolus, exhaust gases passes is configured as between described urceolus and oil feed passage, described preheater is provided with the gas approach and exhanst gas outlet that communicate with described exhaust gases passes, described preheater is also provided with the oil plant import that communicates with described oil feed passage and oil plant exports; Described gas approach is connected by the outlet of described flue with described combustion chamber, and described exhanst gas outlet is connected with the import of described chimney, and described oil plant import is connected with the outlet of described head tank; Bottom or the bottom of described reactor are provided with oil outlet, and the oil-in of described reactor is selected one by valve body and to be exported with the oil outlet of described reactor or the oil plant of described preheater and be connected; Temperature control plate valve is provided with in described flue.
Described reactor being provided with liquid level sensor and safety valve, in described reactor, being provided with the supporting plate for depositing catalyzer.
The pipeline connecting the oil-in of described reactor and the oil outlet of reactor is provided with the first magnetic valve, the pipeline that the oil plant of the oil-in and described preheater that connect described reactor exports is provided with the second magnetic valve, described liquid level sensor is connected with the second magnetic valve with the first magnetic valve, and described first magnetic valve and the second magnetic valve can control to open and close according to the output valve of described liquid level sensor.
Described thermoscope is temperature sensor, and be provided with the setter for fuel metering supply in described burner, described temperature sensor is connected with setter, and described setter can control the fuel duty in fuel device according to the output valve of temperature sensor.
Also comprise the gas phase catalysis device be arranged between described reactor and condenser, described gas phase catalysis device comprises reaction chamber and is located at the catalytic bed in described reaction chamber, described reaction chamber is connected with the import of described condenser with the vapour outlet of described reactor respectively, described reaction chamber offers and can open or airtight door body, described catalytic bed passes in and out described reaction chamber by described door body.
Also comprise fuel oil drum, be provided with import and outlet, the import of described fuel oil drum is connected with the oil outlet of described oil-gas separator, and the outlet of described fuel oil drum is connected with described burner internal.
Also comprise voltate regulator, spark arrester and gas-holder, be equipped with import and outlet, described air water separator is provided with air outlet, the air outlet of described air water separator is connected with the import of described gas-holder, the outlet of described gas-holder is connected with the import of described spark arrester, the outlet of described spark arrester is connected with the import of voltate regulator, and the outlet of described voltate regulator is connected with described burner internal;
Described condenser comprises the one section of condenser and two sections of condensers that are provided with import and outlet, described oil-gas separator comprises and is provided with import, one section of oil-gas separator of oil outlet and air outlet and two sections of oil-gas separators, the import of described one section of condenser is connected with the vapour outlet of described reactor, the outlet of described one section of condenser is connected with the import of described one section of oil-gas separator, the air outlet of described one section of oil-gas separator is connected with the import of described two sections of condensers, and the outlet of described two sections of condensers is connected with the import of described two sections of oil-gas separators; The import of described air water separator is connected with the air outlet of described two sections of oil-gas separators.
The present invention has following beneficial effect compared with prior art:
(1) waste lubricating oil of the present invention produces the method for diesel oil, comprises in waste lubricating oil, adding catalyzer being heated to 180-410 DEG C, the cut condensation steamed at the temperature disclosed above is obtained oil phase thing is refining obtains diesel oil; Described catalyzer is made up of the component of following weight percent: ferric oxide 1-10%, magnesium oxide 1-10%, γ-Al
2o
3and/or η-Al
2o
320-40%, calcium oxide 3-20%, silicon-dioxide 20-40%.
Cracking catalyst contains B acid site and L acid site, wherein L acid site is arranged in catalyst substrates, Main Function promotes that macromolecule hydrocarbon cracking is medium sized hydrocarbon molecules, but the L acid site of excessive concentration easily causes dehydrogenation, condensation reaction, causes carbonization; B acid site is mainly distributed in photocatalyst crystals, can form carbonium ion, then makes the cracking hydrocarbon of contact carbonium ion become small molecules hydro carbons.B acid site concentration in usual cracking catalyst is higher than L acid site and both concentration is difficult to adjustment, therefore waste lubricating oil produces diesel oil is all make waste lubricating oil pyrolytic cracking under catalyst action form the multiple hydro carbons of differing molecular size usually, by the sepn process such as fractionation, extraction, the diesel component in hydro carbons is extracted again, not only complex manufacturing, consume energy high, pollute large, and diesel yield is very low, a large amount of waste lubricating oil cannot be converted into diesel oil effectively, but transforms in order to the low small molecules hydro carbons of utilization ratio.The application applicant finds after deliberation by the γ-Al of the magnesium oxide of the ferric oxide of 1-10wt%, 1-10wt%, 20-40wt%
2o
3and/or η-Al
2o
3, the calcium oxide of 3-20wt% and 20-40wt% the catalyzer of silica component composition heat at 180-410 DEG C after, catalytic inner divides B acid site meeting dehydroxylation, this part B acid site is converted into L acid site then, thus the concentration in L acid site is improved greatly, this adjustment simultaneously also makes the distribution in B acid site and L acid site on catalyzer more even; Waste lubricating oil is under the effect of this kind of catalyzer, and heavy hydrocarbon is wherein C by cracking
11-C
22the hydro carbons of size, only generates the small molecules hydro carbons of seldom amount, C simultaneously
11-C
22hydro carbons is the component of diesel oil, boiling point is within the scope of 200-390 DEG C, therefore the cracking temperature that the hydro carbons be cracked into is easy at 180-410 DEG C is distilled out, be separated after the material condensation distilled under said temperature through simple, oil phase thing is the thick oil comprising high-content diesel component, more this thick oil is carried out the simple refining high-quality diesel oil product namely obtaining directly using.The diesel component that this kind of method obtains can reach the high yield of more than 85%, and technique is simple, save energy, avoids the problem that existing technique can produce a large amount of waste liquor contamination environment, process cycle is long, efficiency is low, diesel yield is low.
(2) waste lubricating oil of the present invention produces the method for diesel oil, and the temperature of described heating is 340-370 DEG C.The catalytic cracking using catalyzer to carry out waste lubricating oil in this temperature section can improve the yield of diesel component further, thus make more waste lubricating oil can effectively be changed into diesel product for.
(3) waste lubricating oil of the present invention produces the method for diesel oil, and described heat-processed is slow temperature-rise period, and temperature rise rate is 0.3-3 DEG C/min.Waste lubricating oil is the poor conductor of heat, slowly heats up can reduce the coking and condensation problem that the waste lubricating oil near heat source occurs because acutely heating up with this speed.
(4) waste lubricating oil of the present invention produces the device of diesel oil, and comprise reactor, be provided with oil-in, top or top are provided with vapour outlet; Heating installation, comprises interconnective function unit and heat release parts, and at least part of described heat release parts are arranged in described reactor, or described heat release components interior is connected with reactor inside; Condenser, is provided with import and outlet, and the import of described condenser is connected with the vapour outlet of described reactor; Oil-gas separator, is provided with import, air outlet and oil outlet, and the import of described oil-gas separator is connected with the outlet of described condenser; Air water separator, comprises import and water outlet, and the import of described air water separator is connected with the air outlet of described oil-gas separator; Also comprise the thermoscope for measuring described reactor temperature, the temperature-sensitive position of described thermoscope is arranged in described reactor.
Adopt said apparatus, first waste lubricating oil to be sent in reactor and to add catalyzer, by observing the temperature of thermoscope display and controlling heating installation, by heat release parts, the waste lubricating oil in reactor is slowly heated to 180-410 DEG C, the steam steamed in reactor is entered in condenser by pipeline and carries out condensation, after condensation product enters oil-gas separator successively and is separated in air water separator, obtain oil phase thing and be gas oil, after gas oil is refining, be diesel product.Use production equipment of the present invention in the manner described above, diesel yield can be made to reach more than 85%, and waste lubricating oil obtains and effectively utilizes.And production equipment of the present invention is simple, technical process is short, the efficiency of producing diesel oil with waste lubricating oil is very high, is suitable for wide popularization and application.
(5) waste lubricating oil of the present invention produces the device of diesel oil, the oil phase thing that the steam exported by reactor contains is not necessarily diesel component completely, a certain amount of macromolecule hydrocarbon may be contained in the inside, condensation is carried out again after making hydrocarbon vapours be introduced into the further catalytic cracking of gas phase catalysis device, the content of diesel component in steam can be improved, thus further increase the yield of diesel component.
(6) waste lubricating oil of the present invention produces the device of diesel oil, and in described heating installation, described function unit is burner, and described heat release parts are the combustion chamber being positioned at described reactor; Described production equipment also comprises chimney, and the import of described chimney is connected with the outlet of described combustion chamber through reactor wall, and the exit of described chimney is provided with smoke purifier.Also comprise the head tank, flue and the preheater that are provided with outlet; Described preheater comprises urceolus and is arranged at the oil feed passage in described urceolus, exhaust gases passes is configured as between described urceolus and oil feed passage, described preheater is provided with the gas approach and exhanst gas outlet that communicate with described exhaust gases passes, described preheater is also provided with the oil plant import that communicates with described oil feed passage and oil plant exports; Described gas approach is connected by the outlet of described flue with described combustion chamber, and described exhanst gas outlet is connected with the import of described chimney, and described oil plant import is connected with the outlet of described head tank; Bottom or the bottom of described reactor are provided with oil outlet, and the oil-in of described reactor is selected one by valve body and to be exported with the oil outlet of described reactor or the oil plant of described preheater and be connected; Temperature control plate valve is provided with in described flue.
Oil plant in burner to be sprayed in combustion chamber and ignition within it by nozzle, the oil plant in the flue gas heating reactor that burning produces, and remaining flue gas is discharged by chimney, and smoke purifier is for removing pellet in flue gas and sulfur-bearing nitrogenous gas.
Further, when oil plant in reactor is sufficient, the oil plant of reactor oil outlet is looped back in reactor, form the circulation of oil plant in reactor, oil plant is fully mixed, decreases oil plant local superheating in still and the problem of carbonization occurs, decreasing the catalyzer lost because of local superheating carbonization, decrease because the oil plant heat transfer that close-burning causes on combustion chamber and flue outer wall is obstructed problem, and the catalyst recycling in reactor can be made by this oil plant circulation; Because the material in reactor is gone out by evaporation continually, when liquid level is lower, the oil plant in preheater can be supplemented in reactor; Oil plant in preheater comes from the oil plant dewatered in head tank, and in combustion chamber, remaining high-temperature flue gas passes into the exhaust gases passes of preheater to heat the oil plant of dehydration of preheater through flue.
Temperature control plate valve in flue for controlling the smoke which in flue, to control the Heating temperature of preheater; When in preheater, temperature does not reach preset temp, open temperature control plate valve and discharge more high-temperature flue gas for heating oil plant, when temperature in preheater reaches even higher than preset temp, close temperature control plate valve to maintain oil plant in preheater in certain temperature range, preset temp is typically chosen in 180-220 DEG C, with the residual water-content gasified in oil plant, avoid moisture to bring in reactor and cause air pressure to raise the problem with temperature fluctuation instantaneously.
(7) waste lubricating oil of the present invention produces the device of diesel oil, described reactor being provided with liquid level sensor and safety valve, being provided with the supporting plate for depositing catalyzer in described reactor.Also comprise fuel oil drum, be provided with import and outlet, the import of described fuel oil drum is connected with the oil outlet of described oil-gas separator, and the outlet of described fuel oil drum is connected with described burner internal.
Because the material in reactor is gone out by evaporation continually, therefore need the liquid level of being observed by liquid level sensor in still, when liquid level is lower, waste lubricating oil can be supplemented in still.Safety valve can discharge gas with pressure release in good time, avoids blasting, provides safety control.Catalyzer is placed on supporting plate, and the content of beginning step of reaction still inner catalyst can be made higher, and reaction efficiency is higher, avoids beginning reaction time catalizer and easily sinks and cause still inner catalyst concentration not high, the problem that reaction efficiency is low.The gas oil that waste lubricating oil obtains after reaction, condensation, gas-oil separation to can be passed through after filter directly as oil fuel for burner.
Accompanying drawing explanation
In order to make content of the present invention more easily be understood, the present invention is further detailed content of the present invention with embodiment by reference to the accompanying drawings;
Fig. 1 is the structural representation that waste lubricating oil of the present invention produces diesel device;
Fig. 2 is the structural representation that the waste lubricating oil with head tank, flue and preheater of the present invention produces diesel device;
Fig. 3 is the structural representation that the waste lubricating oil with gas phase catalysis device, head tank, flue and preheater of the present invention produces diesel device;
Fig. 4 is the structural representation of gas phase catalysis device of the present invention;
Fig. 5 is the structural representation that the waste lubricating oil with gas phase catalysis device, flue, liquid level sensor, safety valve, head tank, fuel oil drum, voltate regulator and spark arrester of the present invention produces diesel device;
Wherein Reference numeral is: 1-reactor, 2-oil-in, 3-vapour outlet, 4-heating installation, 5-condenser, 6-oil-gas separator, 7-air water separator, 8-temperature sensor, 9-gas phase catalysis device, 10-reaction chamber, 11-door body, 12-burner, 13-combustion chamber, 14-preheater, 15-flue, 16-chimney, 17-smoke purifier, 18-temperature control plate valve, 19-head tank, 20-oil outlet, 21-liquid level sensor, 22-safety valve, 23-supporting plate, 24-first magnetic valve, 25-second magnetic valve, 26-fuel oil drum, 27-voltate regulator, 28-spark arrester, 29-gas-holder, 30-dewatering unit, 31-filtering net, 32-wash water valve.
Embodiment
Embodiment 1
Mix add 2.5kg catalyzer in 5t waste lubricating oil after, slowly heat up with the speed of 0.7 DEG C/min and remain on 180 DEG C, the oil phase obtained after normal-temperature water condensation, gas-oil separation, gas-water separation by the cut steamed at 180 DEG C is gas oil, namely described gas oil obtain diesel product through decolouring, interpolation stablizer and anti-cerate, and the diesel yield that above-mentioned waste lubricating oil produces diesel oil technique is 86%.
Described catalyzer by ferric oxide 1%, magnesium oxide 1%, γ-Al
2o
310%, η-Al
2o
330%, calcium oxide 18% and silicon-dioxide 40% form.
Embodiment 2
Mix add 5kg catalyzer in 5t waste lubricating oil after, slowly heat up with the speed of 1 DEG C/min and remain on 340 DEG C, the oil phase obtained after normal-temperature water condensation, gas-oil separation, gas-water separation by the cut steamed at 340 DEG C is gas oil, namely described gas oil obtain diesel product through decolouring, interpolation stablizer, cetane number improving agent and anti-cerate, and the diesel yield that above-mentioned waste lubricating oil produces diesel oil technique is 88%.
Described catalyzer by ferric oxide 10%, magnesium oxide 1%, γ-Al
2o
340%, calcium oxide 29% and silicon-dioxide 20% form.
Embodiment 3
Mix add 5kg catalyzer in 5t waste lubricating oil after, slowly heat up with the speed of 0.8 DEG C/min and remain on 365 DEG C, the oil phase obtained after normal-temperature water condensation, gas-oil separation, gas-water separation by the cut steamed at 365 DEG C is gas oil, namely described gas oil obtain diesel product through decolouring, interpolation stablizer, cetane number improving agent and anti-cerate, and the diesel yield that above-mentioned waste lubricating oil produces diesel oil technique is 90%.
Described catalyzer by ferric oxide 1%, magnesium oxide 10%, γ-Al
2o
340%, calcium oxide 29% and silicon-dioxide 20% form.
Embodiment 4
Mix add 2g catalyzer in 1kg waste lubricating oil after, slowly heat up with the speed of 3 DEG C/min and remain on 357 DEG C, the oil phase obtained after normal-temperature water condensation, gas-oil separation, gas-water separation by the cut steamed at 357 DEG C is gas oil, namely described gas oil obtain diesel product through decolouring, interpolation stablizer, cetane number improving agent and anti-cerate, and the diesel yield that above-mentioned waste lubricating oil produces diesel oil technique is 87%.
Described catalyzer by ferric oxide 5%, magnesium oxide 8%, η-Al
2o
320%, calcium oxide 27% and silicon-dioxide 40% form.
Embodiment 5
Mix add 11kg catalyzer in 1t waste lubricating oil after, slowly heat up with the speed of 2 DEG C/min and remain on 360 DEG C, the oil phase obtained after normal-temperature water condensation, gas-oil separation, gas-water separation by the cut steamed at 360 DEG C is gas oil, namely described gas oil obtain diesel product through decolouring, interpolation stablizer, cetane number improving agent and anti-cerate, and the diesel yield that above-mentioned waste lubricating oil produces diesel oil technique is 87%.
Described catalyzer by ferric oxide 10%, magnesium oxide 10%, η-Al
2o
335%, calcium oxide 20% and silicon-dioxide 25% form.
Embodiment 6
Mix add 50kg catalyzer in 1t waste lubricating oil after, slowly heat up with the speed of 2.5 DEG C/min and remain on 370 DEG C, the oil phase obtained after normal-temperature water condensation, gas-liquid separation, oily water separation by the cut steamed at 370 DEG C is gas oil, namely described gas oil obtain diesel product through decolouring, interpolation stablizer, cetane number improving agent and anti-cerate, and the diesel yield that above-mentioned waste lubricating oil produces diesel oil technique is 92%.
Described catalyzer by ferric oxide 10%, magnesium oxide 7%, η-Al
2o
340%, calcium oxide 3% and silicon-dioxide 40% form.
Embodiment 7
Mix add 8kg catalyzer in 8t waste lubricating oil after, slowly heat up with the speed of 0.3 DEG C/min and remain on 410 DEG C, by the cut that steams at 410 DEG C through the one section of condensation of 340 DEG C of hot steams, mink cell focus phases and gas gas-phase objects is obtained after one section of gas-oil separation, by gas gas-phase objects through normal-temperature water two sections of condensations, lightweight oil phases is obtained after two sections of gas-oil separation, mink cell focus phases is through decolouring, add stablizer, namely cetane number improving agent and anti-cerate obtain heavy diesel product, lightweight oil phases is through decolouring, add stablizer, namely cetane number improving agent and anti-cerate obtain LIGHT DIESEL OIL product, total diesel yield that above-mentioned waste lubricating oil produces diesel oil technique is 87%.
Described catalyzer by ferric oxide 5%, magnesium oxide 5%, η-Al
2o
335%, calcium oxide 15% and silicon-dioxide 40% form.
Embodiment 8
Mix add 60kg catalyzer in 6t waste lubricating oil after, slowly heat up with the speed of 0.5 DEG C/min and remain on 380 DEG C, by the cut that steams at 380 DEG C through the one section of condensation of 340 DEG C of hot steams, heavies condensation thing and gas gas-phase objects is obtained after one section of gas-liquid separation, by gas gas-phase objects through normal-temperature water two sections of condensations, light condensate is obtained after two sections of gas-liquid separations, be heavy gas oil by the oil phase obtained after the oily water separation of heavies condensation thing, through decolouring, add stablizer, namely cetane number improving agent and anti-cerate obtain heavy diesel product, be light gas oil by the oil phase obtained after light condensate oily water separation, through decolouring, add stablizer, namely cetane number improving agent and anti-cerate obtain LIGHT DIESEL OIL product, total diesel yield that above-mentioned waste lubricating oil produces diesel oil technique is 85%.
Described catalyzer by ferric oxide 5%, magnesium oxide 7%, γ-Al
2o
320%, η-Al
2o
319%, calcium oxide 14% and silicon-dioxide 35% form.
In above-described embodiment, the preparation method of catalyzer is: by ferric oxide, magnesium oxide, titanium dioxide, calcium oxide and γ-Al
2o
3and/or η-Al
2o
3mix formation pre-composition, in pre-composition, add the water being equivalent to premix mass 5-10%, continue mix and be shaped to particle, dry 2-8h at particle being placed in 70-130 DEG C.The preparation method of above embodiment catalyzer is not limited only to aforesaid method, and any method can preparing specific components catalyzer in above embodiment is all applicable to the present invention.
Comparative example 1
1t waste lubricating oil to be loaded in still kettle and the mordenite adding waste lubricating oil weight 0.8% as catalyzer, heating and temperature control is at 150 DEG C, obtain distillate 500kg, to add in stirrer and to add industrial sulphuric acid 5kg, obtaining supernatant liquor 460kg, then supernatant liquor is added in stirrer, the aqueous solution simultaneously 4.6kg sodium hydroxide being mixed with 30% concentration adds in stirrer, stir after 2 hours and leave standstill 3 hours again, obtain supernatant liquor and be diesel oil, diesel yield is 38%.
Comparative example 2
1t waste lubricating oil to be loaded in still kettle and the mordenite adding waste lubricating oil weight 1.5% as catalyzer, heating and temperature control is at 360 DEG C, obtain distillate 600kg, to add in stirrer and to add industrial sulphuric acid 9kg, obtaining supernatant liquor 540kg, then supernatant liquor is added in stirrer, the aqueous solution simultaneously 8kg sodium hydroxide being mixed with 30% concentration adds in stirrer, stir after 3 hours and leave standstill 5 hours again, obtain supernatant liquor and be diesel oil, diesel yield is 41%.
The production equipment of the diesel oil method of being produced by waste lubricating oil that embodiment 1-8 processing method uses, its structure as shown in Figure 1, comprise reactor 1, be provided with oil-in 2, top or bottom are provided with vapour outlet 3, the position of described oil-in 2 can be arranged as required, and in the present embodiment, described oil-in 2 and vapour outlet 3 are all arranged on the top of reactor 1.Heating installation 4, comprises interconnective function unit and heat release parts, and at least part of described heat release parts are arranged in described reactor 1 or described heat release components interior is connected with described reactor 1 inside.Wherein, the particular type of described function unit and heat release parts can be selected according to actual needs, in prior art, any equipment that can control heat release parts release of heat size in burner 12 all can be used as function unit use, anyly can all can be used as heat release parts and use by the equipment of material in releases heat reacting by heating still 1, in the present embodiment, described function unit is burner 12, described burner 12 can select any type of the prior art, the gradual burner 12 of the preferred double fuel of the present embodiment two sections of fire, described heat release parts are the combustion chamber 13 being positioned at described reactor 1, described combustion chamber 13 is the pipeline of a large diameter, described burner 12 is connected with the import of combustion chamber 13, described production equipment also comprises chimney 16, and the import of described chimney 16 is connected with the outlet of described combustion chamber 13 through reactor 1 wall, and the exit of described chimney 16 is provided with the smoke purifier 17 for removing particulate matter in flue gas, sulfur-bearing, nitrogenous substances.Condenser 5, be provided with import and outlet, the import of described condenser 5 is connected with the vapour outlet 3 of described reactor 1, described condenser 5 can select any type of the prior art as required, in the present embodiment, described condenser 5 is the inner structure being provided with water of condensation runner and material flow path, indirectly cools the evaporant from reactor 1 in material flow path by water of condensation, and described import and outlet are arranged on the both sides of described condenser 5.Oil-gas separator 6, be provided with import, air outlet and oil outlet, the import of described oil-gas separator 6 is connected with the outlet of described condenser 5, described oil-gas separator 6 can select any type of the prior art as required, in the present embodiment, described oil-gas separator 6 is the tank body that inner chamber is very large, and described import is arranged on the middle part of oil-gas separator 6, described air outlet is arranged on the top of oil-gas separator 6, and described oil outlet is arranged on the bottom of oil-gas separator 6.Air water separator 7, comprise import and water outlet, the import of described air water separator 7 is connected with the air outlet of described oil-gas separator 6, described air water separator 7 can select any type of the prior art as required, in the present embodiment, described air water separator 7 has flowing water Valve and the transparent cylindrical shell of sidewall for bottom, and described import is arranged on the top of air water separator 7.For measuring the thermoscope of temperature in described reactor 1, the temperature-sensitive position of described thermoscope is arranged in described reactor 1, the type of thermoscope can be selected as required, in the present embodiment, described thermoscope is temperature sensor 8, the setter for fuel metering supply is provided with in described burner 12, temperature threshold is stored in described setter, described temperature sensor 8 is connected with setter, described setter can control the fuel duty in fuel device according to the output valve of temperature sensor 8, when the temperature value that temperature sensor 8 exports exceedes the temperature threshold in setter, setter control combustion device 12 reduces supply of fuel, when the temperature value that temperature sensor 8 exports is no more than the temperature threshold in setter, setter control combustion device 12 continues supply fuel, can accurately control temperature in reactor 1 thus.
When using said apparatus to produce diesel oil according to method described in embodiment 1-8, first waste lubricating oil to be sent in reactor 1 and to add corresponding catalyzer, by combustion chamber 13 transferring heat the waste lubricating oil in reactor 1 slowly to be heated with certain speed by observing temperature control combustion device 12 that temperature sensor 8 shows and to remain on temperature required, the steam steamed in reactor 1 is entered in condenser 5 by pipeline and carries out condensation, after condensation product enters oil-gas separator 6 successively and is separated in air water separator 7, obtain oil phase thing and be gas oil, gas oil is through decolouring, add stablizer, namely cetane number improving agent and anti-cerate obtain diesel product after refining.
On the basis of the above, in order to improve final diesel yield further, as shown in Figure 2, the head tank 19, flue 15 and the preheater 14 that are provided with outlet is also comprised; Described preheater 14 comprises urceolus and is arranged at the oil feed passage in described urceolus, exhaust gases passes is configured as between described urceolus and oil feed passage, described preheater is provided with the gas approach and exhanst gas outlet that communicate with described exhaust gases passes, described preheater 14 is also provided with the oil plant import communicated with described oil feed passage and oil plant exports; Described gas approach is connected by the outlet of described flue 15 with described combustion chamber 13, and described exhanst gas outlet is connected with the import of described chimney 16, and described oil plant import is connected with the outlet of described head tank 19; Bottom or the bottom of described reactor 1 are provided with oil outlet 20, and the oil-in 2 of described reactor 1 is selected one by valve body and to be exported with the oil outlet 20 of described reactor 1 or the oil plant of described preheater 14 and be connected; Temperature control plate valve 18 is provided with in described flue 15, in the present embodiment, connect on the oil-in 2 of described reactor 1 and the pipeline of the oil outlet 20 of reactor 1 and be provided with the first magnetic valve 24, the pipeline that the oil plant of the oil-in 2 and described preheater 14 that connect described reactor 1 exports is provided with the second magnetic valve 25, described liquid level sensor 21 is connected with the second magnetic valve 25 with the first magnetic valve 24, and described first magnetic valve 24 and the second magnetic valve 25 can control to open and close according to the output valve of described liquid level sensor 21.When oil mass in reactor 1 is sufficient, open the first magnetic valve 24, close the second magnetic valve 25 simultaneously, oil plant is constantly circulated, equalization temperature, avoid coking in still, when in reactor 1 during low on fuel, open the second magnetic valve 25, close the first magnetic valve 24 simultaneously, preheater 14 supplements through heating and the waste lubricating oil dewatered in time in reactor 1, avoid dryouting, the oil plant that dewatered in head tank 19 is preheated to 180-220 DEG C by preheater 14, the residual water-content that can be gasified totally in oil plant, oil plant is avoided to enter reaction, moisture transient evaporation after the 1 and pressure in still is raised, and the oil plant of preheating effectively can reduce the temperature fluctuation in reactor 1, thus reduce the negative impact of temperature fluctuation to reaction.
As shown in Figure 3-4, described production equipment also comprises the gas phase catalysis device 9 be arranged between described reactor 1 and condenser 5, the catalytic bed that described gas phase catalysis device 9 comprises reaction chamber 10 and is located in described reaction chamber 10, described reaction chamber 10 is connected with the import of described condenser 5 with the vapour outlet 3 of described reactor 1 respectively, described reaction chamber 10 offers and can open or airtight door body 11, described catalytic bed passes in and out described reaction chamber 10 by the position offering this body 11, diesel yield can be improved after the further catalytic cracking of the gas phase catalysis device 9 of the material evaporated by reactor 1 through being built-in with beds, the gas phase catalyst in gas phase catalysis device 9 reaction chamber 10 can be changed in time by the door body 11 that can open or seal.In the present embodiment, the inwall of described door body 11 is outwardly shaped to the shape of truncated rectangular pyramids, the outer side wall of this truncated rectangular pyramids is provided with gasket, accordingly, described reaction chamber 10 arranges a body 11 place and is inwardly recessed, when described door body 11 is closed, the recess of reaction chamber 10 and the outer side wall of described door body 11 truncated rectangular pyramids are tightly connected by described gasket, and described gasket is preferably asbestos packing, graphite pads or SW with outside ring.Also comprise pressing close to the first fastening assembly that a body 11 hinged place is arranged, described first fastening assembly comprises first groove relative with this through hole and the first bolt with nut on through hole on described door body 11, reaction chamber 10 sidewall.Time airtight, will the first bolt of band nut through after through hole, its front end is stretched in the first groove fixing, then nut screwing clamping can be fastened a body 11 hinged, make it seal; When beating opening door body 11, only nut need be unscrewed rear extraction first bolt to the openable degree of door body 11.Wherein, internal thread can be set in the first groove, the first bolt front end is tightened in the first groove, or use pin to be fixed through the first bolt front end and the first groove; Also comprise the second fastening assembly, be arranged at one side relative with door body 11 hinged place on described door body 11, described second fastening assembly comprises second groove relative with this open hole and the second bolt with nut on open hole on described door body 11, reaction chamber 10 sidewall.Time airtight, the second bolt of band nut is through open hole, and its front end is stretched in the second groove fixing, nut screwing clamping thus fasten on a body 11 relative with door body 11 hinged place, makes it seal; When beating opening door body 11, only nut need be unscrewed rear extraction second bolt to the openable degree of door body 11, the second bolt also can be made to turn to a body 11 by the opening of open hole can opening degree or directly disassembled by opening by the second bolt; Wherein, internal thread can be set in the second groove, the second bolt front end is tightened in the second groove, or use pin to be fixed through the second bolt front end and the second groove.
On this basis, as shown in Figure 5, also comprise fuel oil drum 26, be provided with import and outlet, the import of described fuel oil drum 26 is connected with the oil outlet of described oil-gas separator 6, and the outlet of described fuel oil drum 26 is connected with described burner 12 inside; The oil product of waste lubricating oil after reaction, condensation, gas-oil separation can directly as fuel for burner.In described fuel oil drum 26, be provided with filtering net 31 between superposed import and the outlet of bottom, for sifting out the impurity particle in oil, and the bottom of described fuel oil drum 26 is provided with wash water valve 32.Also comprise voltate regulator 27 and spark arrester 28, be equipped with import and outlet, the air outlet of described air water separator 7 is connected by the import of gas-holder 29 with spark arrester 28, the outlet of described spark arrester 28 is connected with the import of voltate regulator 27, the outlet of described voltate regulator 27 is connected with described burner 12 inside, and the fuel that the gradual burner 12 of double fuel two sections of fire uses can switch between the geseous fuel that separates of oil plant in fuel oil drum 26 and air water separator 7.When the oil-air pressure that air water separator 7 separates reaches incendivity pressure, burner 12 automatically switches to burning gaseity, and when oil-air pressure is not enough, fuel oil drum 26 is to burner 12 fuel feeding, and now burner 12 automatically switches to oil firing state, described condenser 5 can also comprise the one section of condenser and two sections of condensers that are provided with import and outlet, described oil-gas separator 6 can comprise and is provided with import, one section of oil-gas separator of oil outlet and air outlet and two sections of oil-gas separators, the import of described one section of condenser is connected with the vapour outlet 3 of described reactor 1, the outlet of described one section of condenser is connected with the import of described one section of oil-gas separator, the air outlet of described one section of oil-gas separator is connected with the import of described two sections of condensers, the outlet of described two sections of condensers is connected with the import of described two sections of oil-gas separators, the import of described air water separator 7 is connected with the air outlet of described two sections of oil-gas separators.The cut that high temperature steams obtains heavy gas oil after one section of condensation, one section of gas-oil separation, and the gas phase that one section of gas-oil separation goes out obtains light gas oil after two sections of condensations, two sections of gas-oil separation, obtains diesel product after two kinds of gas oil are refining.Above-mentioned one section of condenser, two sections of condensers, one section of oil-gas separator, two sections of oil-gas separators, air water separator are respectively the common structure of condenser in prior art, oil-gas separator and air water separator, no longer introduce, and also do not mark in accompanying drawing at this.Described reactor 1 is provided with liquid level sensor 21 and safety valve 22, described liquid level sensor 21 and safety valve 22 all select conventional equipment of the prior art, the supporting plate 23 for depositing catalyzer is provided with in described reactor 1, the outer wall of described reactor 1 and gas phase catalyst converter 9 is provided with thermal insulation layer (not marking thermal insulation layer in accompanying drawing), described liquid level sensor 21 is arranged at the top of described reactor 1 sidewall in the present embodiment, described safety valve 22 is arranged at the top of described reactor 1, described supporting plate 23 to be set in parallel in described reactor 1 and to be positioned at the top of described combustion chamber 13.
Although the present invention has carried out detailed elaboration by above-mentioned specific embodiment to it; but; those skilled in the art should be understood that and made on this basis not exceed any form of claims and the change of details, all belong to invention which is intended to be protected.
Claims (15)
1. produce a method for diesel oil with waste lubricating oil, comprise the steps,
(1) in waste lubricating oil, add catalyzer, heat and remain on 180-410 DEG C, the cut steamed under obtaining said temperature;
(2) the oil phase thing described cut condensation obtained is refined;
Described catalyzer is made up of the component of following weight percent: ferric oxide 1-10%, magnesium oxide 1-10%, γ-Al
2o
3and/or η-Al
2o
320-40%, calcium oxide 3-20%, silicon-dioxide 20-40%.
2. method according to claim 1, is characterized in that, the temperature rise rate starting to heat is 0.3-3 DEG C/min.
3. method according to claim 1 and 2, is characterized in that, the temperature of described heating is 340-370 DEG C.
4. method according to claim 3, is characterized in that, described catalyst weight is the 0.05-5% of described waste lubricating oil weight.
5. method according to claim 1 and 2, is characterized in that, described catalyst weight is the 0.05-5% of described waste lubricating oil weight.
6. method according to claim 4, is characterized in that, first described cut fraction section condensation is obtained mink cell focus phases and gas gas-phase objects, then the two sections of condensations of described gas gas-phase objects are obtained lightweight oil phases; Obtain heavy diesel by refining for described mink cell focus phases, obtain LIGHT DIESEL OIL by refining for described lightweight oil phases.
7. the production equipment of method described in any one of claim 1-6, comprises reactor (1), is provided with oil-in (2), and top or top are provided with vapour outlet (3);
Heating installation (4), comprise interconnective function unit and heat release parts, at least part of described heat release parts are arranged in described reactor (1) or described heat release components interior is connected with described reactor (1) inside;
Condenser (5), is provided with import and outlet, and the import of described condenser (5) is connected with the vapour outlet (3) of described reactor (1);
Oil-gas separator (6), is provided with import, air outlet and oil outlet, and the import of described oil-gas separator (6) is connected with the outlet of described condenser (5);
Air water separator (7), comprises import and water outlet, and the import of described air water separator (7) is connected with the air outlet of described oil-gas separator (6);
For measuring the thermoscope of described reactor (1) interior temperature, the temperature-sensitive position of described thermoscope is arranged in described reactor (1);
Described oil-in (2) is arranged on the top of reactor (1).
8. production equipment according to claim 7, it is characterized in that, in described heating installation (4), described function unit is burner (12), and described heat release parts are for being positioned at the combustion chamber (13) of described reactor (1); Described production equipment also comprises chimney (16), the import of described chimney (16) is connected with the outlet of described combustion chamber (13) through reactor wall, and the exit of described chimney (16) is provided with smoke purifier (17).
9. production equipment according to claim 8, is characterized in that, also comprises the head tank (19), flue (15) and the preheater (14) that are provided with outlet; Described preheater (14) comprises urceolus and is arranged at the oil feed passage in described urceolus, exhaust gases passes is configured as between described urceolus and oil feed passage, described preheater is provided with the gas approach and exhanst gas outlet that communicate with described exhaust gases passes, described preheater (14) is also provided with the oil plant import communicated with described oil feed passage and oil plant exports; Described gas approach is connected by the outlet of described flue (15) with described combustion chamber (13), described exhanst gas outlet is connected with the import of described chimney (16), and described oil plant import is connected with the outlet of described head tank (19); The bottom of described reactor (1) or bottom are provided with oil outlet (20), and the oil-in (2) of described reactor (1) is selected one by valve body and to be exported with the oil outlet (20) of described reactor (1) or the oil plant of described preheater (14) and be connected; Temperature control plate valve (18) is provided with in described flue (15).
10. production equipment according to claim 9, it is characterized in that, described reactor (1) being provided with liquid level sensor (21) and safety valve (22), in described reactor (1), being provided with the supporting plate (23) for depositing catalyzer.
11. production equipments according to claim 10, it is characterized in that, the pipeline connecting the oil-in (2) of described reactor (1) and the oil outlet (20) of reactor (1) is provided with the first magnetic valve (24), the pipeline that the oil plant of the oil-in (2) and described preheater (14) that connect described reactor (1) exports is provided with the second magnetic valve (25), described liquid level sensor (21) is connected with the second magnetic valve (25) with the first magnetic valve (24), described first magnetic valve (24) and the second magnetic valve (25) can control to open and close according to the output valve of described liquid level sensor (21).
12. production equipments according to Claim 8 described in-11 any one, it is characterized in that, described thermoscope is temperature sensor (8), the setter for fuel metering supply is provided with in described burner (12), described temperature sensor (8) is connected with setter, and described setter can control the fuel duty in fuel device according to the output valve of temperature sensor (8).
13. production equipments according to claim 12, it is characterized in that, also comprise the gas phase catalysis device (9) be arranged between described reactor (1) and condenser (5), the catalytic bed that described gas phase catalysis device (9) comprises reaction chamber (10) and is located in described reaction chamber (10), described reaction chamber (10) is connected with the import of described condenser (5) with the vapour outlet (3) of described reactor (1) respectively, described reaction chamber (10) offers and can open or airtight door body (11), described catalytic bed passes in and out described reaction chamber (10) by described door body (11).
14. production equipments according to claim 13, it is characterized in that, also comprise fuel oil drum (26), be provided with import and outlet, the import of described fuel oil drum (26) is connected with the oil outlet of described oil-gas separator (6), and the outlet of described fuel oil drum (26) is connected with described burner (12) inside.
15. production equipments according to claim 14, it is characterized in that, also comprise voltate regulator (27), spark arrester (28) and gas-holder (29), be equipped with import and outlet, (7) are provided with air outlet with described air water separator, the air outlet of described air water separator (7) is connected with the import of described gas-holder (29), the outlet of described gas-holder (29) is connected with the import of described spark arrester (28), the outlet of described spark arrester (28) is connected with the import of voltate regulator (27), the outlet of described voltate regulator (27) is connected with described burner (12) inside,
Described condenser (5) comprises the one section of condenser and two sections of condensers that are provided with import and outlet, described oil-gas separator (6) comprises and is provided with import, one section of oil-gas separator of oil outlet and air outlet and two sections of oil-gas separators, the import of described one section of condenser is connected with the vapour outlet (3) of described reactor (1), the outlet of described one section of condenser is connected with the import of described one section of oil-gas separator, the air outlet of described one section of oil-gas separator is connected with the import of described two sections of condensers, the outlet of described two sections of condensers is connected with the import of described two sections of oil-gas separators, the import of described air water separator (7) is connected with the air outlet of described two sections of oil-gas separators.
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| CN201310423492.0A CN103484156B (en) | 2013-08-29 | 2013-09-17 | A kind of waste lubricating oil produces method and the production equipment thereof of diesel oil |
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| CN201310383605 | 2013-08-29 | ||
| CN2013103836059 | 2013-08-29 | ||
| CN201310423492.0A CN103484156B (en) | 2013-08-29 | 2013-09-17 | A kind of waste lubricating oil produces method and the production equipment thereof of diesel oil |
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| CN201320575114.XU Expired - Fee Related CN203582814U (en) | 2013-08-29 | 2013-09-17 | Production device for producing diesel by using waste lubricating oil |
| CN201310423492.0A Expired - Fee Related CN103484156B (en) | 2013-08-29 | 2013-09-17 | A kind of waste lubricating oil produces method and the production equipment thereof of diesel oil |
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| CN106398759B (en) * | 2016-11-19 | 2017-12-22 | 河北天理环保科技有限公司 | Waste lubricant oil regeneration and production diesel device |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5306419A (en) * | 1993-08-05 | 1994-04-26 | Texaco Inc. | Used lubricating oil reclaiming |
| CN101531948A (en) * | 2009-04-10 | 2009-09-16 | 熊道陵 | New technology for catalytically cracking light diesel oil from waste motor oil |
| CN102226104A (en) * | 2011-05-23 | 2011-10-26 | 大连理工大学 | Method for producing gasoline and diesel by utilizing waste lubricating oil |
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| CN203582814U (en) * | 2013-08-29 | 2014-05-07 | 连力生 | Production device for producing diesel by using waste lubricating oil |
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2013
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5306419A (en) * | 1993-08-05 | 1994-04-26 | Texaco Inc. | Used lubricating oil reclaiming |
| CN101531948A (en) * | 2009-04-10 | 2009-09-16 | 熊道陵 | New technology for catalytically cracking light diesel oil from waste motor oil |
| CN102226104A (en) * | 2011-05-23 | 2011-10-26 | 大连理工大学 | Method for producing gasoline and diesel by utilizing waste lubricating oil |
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