CN102585896A - Automatic continuous production process for producing diesel oil with waste oil through catalytic cracking method - Google Patents
Automatic continuous production process for producing diesel oil with waste oil through catalytic cracking method Download PDFInfo
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Abstract
The invention relates to the technical field of waste oil comprehensive utilization and fuel oil processing, particularly to an automatic continuous production process for producing diesel oil with waste oil through a catalytic cracking method. The production process comprises the following process steps: 1, the waste oil is pretreated; 2, the pretreated waste oil is subjected to hot cracking and catalytic cracking, so as to obtain crude oil, wherein the catalytic cracking comprises liquid-phase catalysis and gas-phase catalysis; 3, the crude oil is fractionated; and 4, the finished product is obtained through refining and filtering. The invention has the advantages that gelatine, asphaltene, sulfide, oxide, unsaturated hydrocarbon and the like can be well removed, so that the finished oil is clear and transparent, has a pure smell, and cannot deteriorate after being stored for a long time; viscosity and pipeline blockage are avoided in the production process, the production process is simple, the conditions are easy to control, the investment is low, the results are quick, the efficiency is high, the use is simple, and the operation is convenient.
Description
Technical field
The present invention relates to waste oil comprehensive utilization and oil fuel processing technique field, particularly a kind of automatic continuous production technology of splitting method waste oil regeneration diesel oil of urging.
Background technology
The oil supply growing tension, price rises steadily, and resource is exhausted day by day, there is some evidence, and the low oil price epoch possibly be gone for ever.In order to alleviate the oil supply anxiety, make full use of Energy resources, energy-saving and emission-reduction, minimizing are polluted, turning waste into wealth becomes a fundamental state policy of country; Make full use of scrap feed material, particularly waste and old oils is carried out catalytic pyrolysis regeneration weight diesel oil, fuel wet goods, can alleviate the China's oil shortage and the growing imbalance between supply and demand of demand; Can promote environmental protection again; Turning waste into wealth, is that the wisdom of country, society, enterprise is selected, and prospect is very wide.But waste and old oil product is of a great variety, complicated component; Quality differs, and catalytic pyrolysis is extremely difficult, and especially catalytic cracking catalyst, catalytic pyrolysis novel process and new installation lack especially; Make the resource utilization of waste and old oils be not in full use, making the best use of everything does not reach desired effects.
Waste and old oils (waste oil) mainly comprises MO (petroleum-type) and vegetable and animals oils (oils), and they are very different on composition.The comprehensive utilization of waste oil at present mainly can be divided into three types, and one type is that waste and old oil product (mineral oils) is carried out being used as low side fuel after the roughing, causes resource utilization to can not get performance, causes the wasting of resources.Another kind of is the oil refining process of continuing to use the big factory of petrochemical industry; Waste oil removal of impurities → the go into still → intensification → waste oil steam that dewaters gets into the thick diamicton of Catalytic Layer → remove → remove thin diamicton → absorption → condensation → s.t. → alkali diesel oil that neutralizes → be deployed into, complex process, and equipment is many; Investment is big, and general producer is difficult to bear.Also have one type to be that waste cooking oil or acidifying oil (oils) are produced biodiesel processes, the someone claims that without soda acid with methyl alcohol and simple distillation has just become qualified biofuel product once, this is to disguise replacement of concept.This method is basic just to be reduced greasy molecular weight, does not also change the carbon-chain structure of molecule, and refining depth and anti-oxidant degree do not reach requirement, and such oil still is original grease still, can't reach the physical and chemical index of diesel oil.The state-of-the-art technology of the comprehensive utilization of present waste and old oils it is said it is short-path distillation or molecular distillation; Both solved color problem, and removed soda acid again and washed problem such as cause pH to exceed standard, resistance to emulsion is defective, but investment had been big; Technical requirements is high, and practicality is not strong.We can say also there is not truly the diesel regenerated continuous production type industrialized unit of waste oil cracking of a cover in the market, so regenerated diesel oil viscosity, density, colourity, flash-point, oxidation-resistance etc. are not up to standard.
Traditional process for treating waste oil is waste oil to be added still kettle directly distill, and the oil content that distills out is made with extra care with bronsted lowry acids and bases bronsted lowry.The oil viscosity that this method is made is big, and density is big, will the oxidation blackening in very short time, and stink and the peculiar smell of oil the inside be difficult to remove, and the processing of acid sludge and waste water and discharge and can cause serious secondary pollution to environment.
Domestic regenerated using about waste and old oil product had many reports, and waste and old oil product is diesel regenerated, oil fuel also has some reports or unofficially report or advertisement, but really gets into practical application or large-scale production seldom.Because oil product regeneration or waste and old oil product is diesel regenerated, the control of oil fuel difficult quality, or quality dissatisfaction or environmental protection have problem, and perhaps the performance of product itself is not good, is difficult to compete with regular petroleum products.
Waste and old oil product produces diesel oil or oil fuel once had some reports; For example; Application number is 97118566.2; Patent name is the apparatus and method of the disclosed a kind of regenerating fuel oil from waste oil of Chinese patent of " apparatus and method of regenerating fuel oil from waste oil ", mainly comprises thermal cracker, is used for that the high boiling hydrocarbon material of cracking becomes lighter lower boiling material so that from viscous substance separate hydrocarbons vapor product; Application number is 03118155.4; Patent name is the disclosed a kind of method of utilizing plastic waste, waste oil and heavy oil mixed pyrolysis to produce oil fuel of Chinese patent of " utilizing plastic waste, waste oil and heavy oil mixed pyrolysis to produce the method for oil fuel "; Mainly be that heavy oil, waste oil and plastic waste are mixed the back by a certain percentage as raw material; Add in the cracking reactor continuously, liquid obtains gasoline, diesel oil and heavy oil through fractionation; Application number is 200410060876.1; Patent name is the disclosed a kind of method that the waste oil refinery is become diesel oil of Chinese patent of " the waste oil refinery becomes the method for diesel oil "; Mainly be in waste oil, to add catalyzer to distill; The light constituent steam that boiling produces adds scavenging agent through condensation, adds stablizer after filtering and gets finished product; Application number is 200510047296.3; Patent name mainly is that catalyst mix waste oil is carried out the normal pressure catalytic pyrolysis in reaction kettle for the disclosed a kind of working method of utilizing waste oil to produce oil fuel of the Chinese patent of " a kind of working method of utilizing waste oil to produce oil fuel "; Application number is 200910226800.4; Patent name is the disclosed a kind of used oil waste oil non-hydro catalytic pyrolysis diesel oil technology of the Chinese patent of " used oil waste oil non-hydro catalytic pyrolysis diesel oil technology ", comprises steps such as one-level thermo-cracking, secondary thermo-cracking, non-hydro catalytic pyrolysis; Application number is 201010160808.8; Patent name mainly is to add cats product, the vitriol oil, breakdown of emulsion for the disclosed a kind of method of utilizing waste oil processing liquid fuel oil of the Chinese patent of " utilizing the method for waste oil processing liquid fuel oil "; Filtering and removing heavy metal and other impurity; Add the diatomite adsorption decolouring again, liquid is separated with solid mixture, add Virahol and separate fuel-displaced and water through press filtration; In isolated oil, add flash point improver, oxidation inhibitor, promptly obtain liquid fuel oil after the modulation.But these methods, technology or device all fail thoroughly to change shortcomings such as waste discharge, contaminate environment, complex procedures, production cost that the classical acid sodafining brings are high, consuming time, power consumption, have such-and-such problem more or less.
Summary of the invention
For solving the problems of the technologies described above; The invention provides that a kind of technology is simple, energy-conserving and environment-protective, running cost is low, efficient is high urges the automatic continuous production technology of splitting method waste oil regeneration diesel oil; This technology can urge the waste oil that splits except that MO, can also urge splitting oils waste oil or the mixture of the two; Comprise nearly all kinds of waste oil; Highly versatile, regenerated weight diesel oil or oil fuel limpid bright, color and luster good, calorific value is high, modest viscosity, good fluidity, flash-point high, meets country or industry standard.
The technical scheme that the present invention adopts is: a kind of automatic continuous production technology of splitting method waste oil regeneration diesel oil of urging comprises following process step: 1) waste oil is carried out pre-treatment; 2) pretreated waste oil is carried out thermo-cracking and catalytic pyrolysis obtains crude oil, wherein catalytic pyrolysis comprises liquid-phase catalysis and gas phase catalysis; 3) crude oil is carried out fractionation; 4) obtain finished product through refining, filtration at last.
Further, said waste oil comprises MO, oils waste oil or the mixture of the two.
Further, said waste oil comprise that used oil, waste lubricating oil, useless gear oil, useless machinery oil, waste hydraulic oil, useless transformer oil, damaged tire are slightly refined oil, slightly oil refining of plastic waste, heavy oil, wax oil, residual oil, coal tar, washing oil, waste cooking oil, acidifying oil, oil-fat plant tankage, useless one or more mixture of deceiving vegetable and animals oils.
Further, pre-treatment is dehydration, decon, the mud that deoils, the matter of removing photoresist, the combination of one or more of deoxidation thing in the said step 1).
Further; Said step 2) for pretreated waste oil is pumped into header tank; Dominant discharge gets in scission reaction still and the gas phase catalytic tower successively, respectively under the effect of liquid-phase catalyst, gas phase catalyst, at 350～550 ° of C; With the waste oil catalytic pyrolysis, obtain approaching the crude oil of diesel oil molecules structure.
Further; Said liquid-phase catalyst is made up of base catalyst, co-catalyst and collaborative regulator, and wherein base catalyst accounts for 10～50% in catalyzer, and co-catalyst accounts for 10～40%; Collaborative regulator accounts for 10～50%; Above per-cent all is weight percentage, and wherein, said base catalyst is one or more the mixture in Aluminum chloride anhydrous, iron(ic)chloride, cupric oxide, aluminum oxide, silicon oxide, Manganse Dioxide, the ZIRCONIUM DIOXIDE 99.5; Said co-catalyst is one or more the mixture in activated alumina, pseudo-boehmite dry glue powder, active silicic acid aluminium, silico-aluminate, sial dry glue powder, macroporous silica gel, the large pore molecular sieve; Said collaborative regulator is one or more the mixture in wilkinite, atlapulgite, zeyssatite, attapulgite, the kaolin.
Further, said gas phase catalyst comprises following component: Y zeolite, high silica ZSM-5 molecular sieve, activated alumina, carrier and sticker, and said gas phase catalyst active ingredient is a Y zeolite; Or the mixture of Y zeolite and high silica ZSM-5 molecular sieve; Said gas phase catalyst staple has silico-aluminate that silicon oxide, aluminum oxide form and rare earth, hydrogen, phosphorus modifying element, and wherein Y zeolite accounts for 10～50% in catalyzer, and the high silica ZSM-5 molecular sieve accounts for 0～20%; Activated alumina accounts for 10～40%; Carrier accounts for 30～70%, and sticker accounts for 10～20%, and above per-cent all is weight percentage.
Further, said step 3) is that above-mentioned catalytic pyrolysis gas is introduced separation column, isolates light constituent through the filler in the tower.About 3～5 meters of fractionation tower height, about 30～60 centimetres of diameter, diesel oil gas is drawn the back from cat head and is got into condensation the condensing surface.
Further, treating process adopts and exempts from the acid-alkali refining agent in the said step 4).
Further, said to exempt from the acid-alkali refining agent be a kind of compound finishing agent, comprises following component: absorption-sinking agent 10～80%; Help active ingredient 5～10%; Cats product 0～10%, nonionogenic tenside 0～10%, cosurfactant 0～5%; Surplus is a diesel oil; Above per-cent all is weight percentage, and wherein, said absorption-sinking agent is one or more the mixture in quadrol, triethylamine, N-alkyl diethylolamine, hexahydroaniline, diethylenetriamine, triethylene diamine, triethylene tetramine, the TEPA; The said active ingredient that helps is one or more the mixture in the carbonic ether of thanomin, trolamine, isopropylamine, N-phenyldiethanol-amine, sulfuric acid vinyl ester, guanidine class; Said cats product is one or more the mixture in the soap, alkyl quaternary ammonium salt, Poly Dimethyl Diallyl Ammonium Chloride, polymethyl acyl-oxygen ethyl-trimethyl salmiac of cationic polymers; Said nonionogenic tenside is one or more the mixture in the tensio-active agent, polyoxyethylene 20 sorbitan monooleate, polyoxyethylene 20 sorbitan trioleate, polyoxyethylene-type nonionogenic tenside, polyoxyethylene nonylphenol nonionogenic tenside of polyoxyethylene sorbitan oleic acid ester class; Said cosurfactant is XU 61518.10, to one or more the mixture in NP, n-Heptyl alcohol, n-Octanol, the sec-n-octyl alcohol.
Further, whole process flow is the process in the automatic continuous production of enclosed space charging and deslagging.
In addition, this technology also comprises waste gas recovery burning, and the flue gas heat recovering step.
The present invention provides a kind of automatic continuous production equipment that splits method waste oil regeneration diesel oil of urging; Its advantage is: can long chain alkane and single branched paraffin be carried out cracking; It is constant to keep naphthenic hydrocarbon, multibranched paraffin and aromatic hydrocarbons; Thereby reduce the condensation point of distillate, make the BO of high condensation point be converted into the LIGHT DIESEL OIL that hangs down condensation point, condensation point is lower than-10 degree.Can remove colloid, bituminous matter, sulfide, oxide compound and unsaturated hydrocarbons etc. well, make processed oil limpid bright, smell is pure, puts for a long time and never degenerates.Thickness not in process of production, blocking pipe not, production technique is simple, condition is easy to control, and less investment, instant effect, efficient is high, uses simple, easy to operate.Because of its continuity has guaranteed the production high-level efficiency; Because of its robotization greatly reduces labour intensity, improved security; Because of utilizing various waste oil, it makes the raw material highly versatile; That bullion oil is made with extra care product oil high-quality is bright because of it; At the uniform velocity to reclaim waste gas oneself heat supply energy-conservation especially because of it; Because of its to waste gas, waste residue, useless very environmental protection of the cigarette comprehensive regulation.
The present invention provides a kind of automatic continuous production technology of splitting method waste oil regeneration diesel oil of urging, and it uses following main device and equipment, and has following obvious characteristic:
1, scission reaction still
The extraordinary Era of reaction kettle material selection is vertical oval tubular, can satisfy the requirement of material maximum temperature, and material forced guiding device is installed, and guarantees that material alternately is heated homogeneous heating.
Reaction kettle is provided with continuously feeding and automatic deslagging device, can material continuously sent into reaction kettle and discharge residue through discharge port.The reaction kettle two ends are equipped with maintenance and observation device.
2, tightness system
Variable-diameter structure is adopted at the reaction kettle two ends, is provided with the static-dynamic sealed structure that automatic multidirectional adjusting combines with the special seal material filling type, and it is excessive to prevent to react gas reactor, good sealing effect.
3, heating system
Be provided with process furnace in the reaction kettle outside, by indirect heating reaction kettle body outer wall.Process furnace is made up of body of heater, fuel burner nozzle, thermal chimney road, fume extractor etc.Process furnace is provided with combustion gas direct heating system and telesecurity heating system, can select type of heating as required.
4, TT&C system
Central control station is set especially, a series of low-voltage electrical facilities such as temperature control loop, frequency transformer and electromechanical equipment start button are housed.Comprise:
(1) combustion gas, fume exhaust system: some intelligence instrument field monitoring temperature are set, and automatic and set(ting)value comparison, output signal to the automatic attemperation of on-the-spot YE, thereby satisfy the material reaction requirement.
(2) heat plenum system: multiple spot heat inlet digital display temperature survey display instrument is set, can opens according to temperature and join thermal valve to guarantee that temperature in the kettle is normal.
(3) electromechanical equipment speed control by frequency variation, the overtemperature instrument is reported to the police.
(4) other temperature element and housing.
5, continuously feeding device
Feed system partly is made up of hermetically sealed speed control by frequency variation automatic feeding machine etc., is provided with and prevents that reaction kettle from returning the gas leakage device, guarantees safety.
6, continuous deslagging device
The deslagging device design is ingenious, is provided with the built-up type drawing mechanism, adopts speed control by frequency variation, guarantees that deslagging is continuous, robotization, and guarantees not have oil and gas leakage.Can open the maintenance reaction kettle.
7, crude oil refining system
Being provided with a whole set of is the serial equipment of high-quality, limpid bright finished diesel fuel with the further processing and refining of crude oil, comprises separation column, interchanger, water cooler, water-and-oil separator, refining stirred pot, removal of impurities tower, decolorizing and refining tower, vacuum buffer tank, purolator etc.
8, combustible exhaust gas recycle device
The flammable mix waste gas that material produces in reaction process is delivered to the fuel burner nozzle use that acts as a fuel after recovery, separation, purifying treatment, can be fully or basic the utilization reclaim gas and heat and do not need extra fuel, energy-conservation greatly.
9, fume extractor
Flue gas is drawn by front top is concentrated after repeatedly utilizing in the burner hearth, is provided with fume extractor at furnace roof, is made up of flashboard, temperature element, air distribution valve, and flue gas is drawn through heat recuperation and emptying after repeatedly purifying, and is pollution-free fully.
A kind of automatic continuous production technology of splitting method waste oil regeneration diesel oil of urging provided by the invention is characterized in that comprising following clear superiority and characteristic:
1, charging serialization
Be provided with " oil gas automatic braking device ", material can be sent into reaction kettle continuously hermetically, stops air admission to be in the reaction kettle of the condition of high temperature simultaneously, has solved conventional art and can only be have at normal temperatures packed into material is disposable, a difficult problem that can not charging in the reaction.Adopt uninterrupted fed technology to improve plant factor and production efficiency greatly, guaranteed the oil product homogeneity.
2, deslagging robotization
Continuous discharging slag is a gordian technique, and can it is related to really realize uninterrupted production.This device is well-designed association type echoes with continuously uninterrupted feeder from the dynamic seal slag off apparatus mutually, can under hot conditions, cut off air, realizes uninterrupted deslagging, thereby reaches limit charging truly, the continuous production of limit deslagging.
3, control instrumentsization
Accurate in order to guarantee production operation, relevant working condition and key position are provided with digital instrument, and, have improved the controllability of operation, the promptness of response greatly these data centralization management and feedback.
4, raw material is extensively changed
Traditional refining equipment can only use single raw material basically, big limitations usage ratio of equipment, often be forced to stop production because of there is lack of raw materials.This device can use plurality of raw materials, as: used oil, waste lubricating oil, useless gear oil, useless machinery oil, waste hydraulic oil, useless transformer oil, damaged tire slightly refine oil, slightly oil refining of plastic waste, heavy oil, wax oil, residual oil, coal tar, washing oil, waste cooking oil (being commonly called as sewer oil, hogwash fat, swill oil), acidifying oil, oil-fat plant tankage, all kinds of waste oil fabricate fuel of useless black plant-animal wet goods is oily.
5, twoly urge high yield
Adopt two splitting twoly to urge technology, promptly thermo-cracking and catalytic pyrolysis, liquid-phase catalysis and gas phase catalysis carry out simultaneously.Because raw material is formed complicated; Molecular weight is big, and it is not enough only depending on thermo-cracking, must carry out catalytic pyrolysis; Promptly take the catalytic way will be than the macromole chain rupture; Change its molecular weight, make it to reach basically the carbon-chain structure of diesel oil C14～18, about 230 molecular weight, can improve yield and oil quality greatly like this.
6, energy-conservationization of heating
Owing to adopted the continuous reaction process of uninterrupted charging, so can produce non-condensable gas continuously equably, normally can satisfy the self-continuously needs that heat when producing basically after fuel-displaced, do not need extra fuel, energy-conservation greatly.
7, discharging environmental protectionization
The non-condensable gas that produces in the production is sent into pot arch burning, clean hygiene, energy-conserving and environment-protective after exhaust processor is handled.Flue gas can reach the GB13271-2001 emission standard of air pollutants for boilers through " gas cleaning jar " purifying treatment.Waste residue can further be processed into industrial carbon black or flyash, accomplishes pollution-free zero release basically.
8, production safetyization
Key position in easy fault and accident is provided with the double insurance safety apparatus pointedly, can remove the dangerous condition automatically.Type of heating adopts the long-range heating of indirect type, without naked light, when system breaks down, closes and send hot device to get final product the instantaneous trip heating source, guarantees security of system.In addition, because material is progressively to add reaction kettle, do not have a lot of material accumulation in the reaction kettle, security improves greatly.
9, the flexibility of heating
Reaction kettle is heated and is designed with two cover systems:
(1) exempts from the long-range heating method of naked light.Utilize the non-condensable gas that self produces in the oil refining process independently heating in the burner, be transported in the reaction kettle stove and heat to reaction kettle.Its advantage is to exempt from the naked light reaction kettle to heat, and equipment is more durable, production is safer.
(2) direct naked light heating method in the stove.Let flame directly reaction kettle heated, designed flame distributor especially, can not let the direct contact reacts kettle of naked light itself, thereby guarantee the wearing quality of reaction kettle.Its advantage is that HU is high, need not increase independently roasting kiln and defeated hot system, reduces investment outlay.
Above-mentioned design can be used separately or mix use, has fabulous complementarity and handiness, than other single long-range heating modes bigger advantage is arranged, and is domestic and international initiative.
10, production high efficiency
Serialization is produced and have been saved that normal temperature is reinforced, the time of deslagging and progressively heat up, the slow time loss of cooling, production efficiency improves greatly.
11, oil product high quality
Adopt new catalyst and composite decoloration preservative, the regenerated oil product is limpid bright, and good taste, is never degenerated at the look that remains unchanged for a long period of time.
12, operation is easily changed
Taked power feed, automatic sludge discharge, automatically handle waste gas, automatically dewater removal of impurities, add the agent brand-new design that has robot control system(RCS) such as refining automatically, labour intensity reduces greatly.
13, durableization of equipment
The continous way appliance arrangement is heated evenly, has avoided long-time localized hyperthermia, and in addition, material stock is few in the device, and machine utilization is little, has improved the work-ing life of device greatly.
The automatic continuous production equipment that splits method waste oil regeneration diesel oil of urging provided by the invention is multifunctional equipment and the technology of utilizing all kinds of waste oil regeneration diesel oil, oil fuel, without soda acid, utilizes the new technology and the equipment of fixed-bed catalytic cracking, decolouring, deodorization.Shortcomings such as the waste discharge that the classical acid sodafining brings, environmental pollution, complex procedures, production cost are high, consuming time, power consumption have not only thoroughly been changed; And can improve the quality of products greatly and production capacity, practice thrift cost, really accomplish pollution-free zero release; The protection environment; Turn waste into wealth, make the best use of everything, benefit the nation and the people.This equipment all-weather is produced, closed clean operation, and produce oil is fast, oil is good, and the waste oil transformation efficiency reaches 80～90%, no three wastes non-secondary pollution in the production process.
In sum, the automatic continuous production equipment that splits method waste oil regeneration diesel oil of urging of the present invention has simple to operate, energy-conserving and environment-protective, running cost is low, efficient is high beneficial effect.The waste and old oils wide material sources of automatic production line main raw material of the present invention help environmental protection, can effectively alleviate the degree of dependence of the energy to oil.
Embodiment
Embodiment 1:
The preparation gas phase catalyst
With dual-purpose rare earth ion and 30 kilograms in the former powder of hydrogen ion metathetical Y zeolite REHY, 5 kilograms of high silica ZSM-5 molecular screen primary powders, 15 kilograms of activated aluminas, 60 kilograms of wilkinites, cross 120 mesh sieves, mechanical stirring; Mix; Mixed powder and the sodium silicate binder for preparing are mediated for 15 kilograms, and control pigment mass ratio is 0.55: 1, fully mediates after the extrusion moulding of screw rod banded extruder, pelletizing; Dry under the room temperature; 120 ° of C are down after dry 3 hours, roasting 5 hours under 600 ° of C under oxygen atmosphere, and making diameter is the cylindric gas phase catalyst particle of 4mm.
The preparation liquid-phase catalyst
27 kilograms of Manganse Dioxide, 25 kilograms of activated aluminas and kaolin are pulverized for 48 kilograms, and mechanical stirring mixes, and crosses 200 mesh sieves, and oven dry is 1 hour under 100 ° of C, makes liquid-phase catalyst.
The acid-alkali refining agent is exempted from preparation
In reaction kettle, add 40 kilograms of diesel oil; Add 3 kilograms of 210 kilograms of diethylenetriamines, 32 kilograms of sulfuric acid vinyl esters, 29 kilograms of polymethyl acyl-oxygen ethyl-trimethyl salmiacs, 25 kilograms of polyoxyethylene 20 sorbitan monooleates and XU 61518.10s more successively; At the uniform velocity stirred 30 minutes, and made and exempt from the acid-alkali refining agent.
The first gas phase catalyst of in the gas phase catalysis tower, packing into.With used oil after pre-treatment such as dehydration, decon, the mud that deoils, the matter of removing photoresist, deoxidation thing; Pump into header tank, dominant discharge is put into the scission reaction still, and then entering is equipped with in the gas phase catalysis tower of gas phase catalyst; Promptly respectively under the effect of liquid-phase catalyst and gas phase catalyst; At 380～430 ° of C,, approach the crude oil of diesel oil molecules structure with formation with the used oil catalytic pyrolysis.The cracked oil steam that comes out from the gas phase catalysis tower gets into high about 3.5 meters, and in the about 40 centimetres separation column still of diameter, the diesel oil gas that distills out through inner-tower filling material is drawn the back from cat head and got into condensation the condensing surface; After oily water separation, import refining stirred pot, under the effect of exempting from the acid-alkali refining agent, fully stirred 3～10 minutes; After leaving standstill 5～10 minutes; Tell lower floor's residue, the upper strata oil product that obtains obtains refining finished product after filter filters.It is faint yellow that finished product is, and clarification is almost tasteless, can be used as oil fuel.Through measuring density 853kg/m
3, kinematic viscosity 7.0mm
2/ s, condensation point-10 ° C, 55 ° of C of close flash point, acidity 6mgKOH/100mL, 1 grade of copper corrosion, No. 2.5, colourity, calorific value>=10500 kcal/kg.
Embodiment 2:
The preparation gas phase catalyst
To cross 120 mesh sieves, mechanical stirring with 28 kilograms in the former powder of hydrogen ion metathetical Y zeolite HY, 15 kilograms of high silica ZSM-5 molecular screen primary powders, 20 kilograms of activated aluminas, 50 kilograms of kaolin; Mix; Mixed powder and the pseudo-boehmite sol adhesive for preparing are mediated for 16 kilograms, and control pigment mass ratio is 0.5: 1, fully mediates after the extrusion moulding of screw rod banded extruder, pelletizing; Dry under the room temperature; 120 ° of C are down after dry 3 hours, roasting 5 hours under 600 ° of C under oxygen atmosphere, and making diameter is the cylindric gas phase catalyst particle of 4mm.
The preparation liquid-phase catalyst
30 kilograms of Aluminum chloride anhydrouss, 25 kilograms in active silicic acid aluminium and zeyssatite are pulverized for 45 kilograms, and mechanical stirring mixes, and crosses 200 mesh sieves, and oven dry is 1 hour under 100 ° of C, makes liquid-phase catalyst.
The acid-alkali refining agent is exempted from preparation
In reaction kettle, add 35 kilograms of diesel oil; Add 240 kilograms of N-alkyl diethylolamine, 28 kilograms of isopropylamine, 24 kilograms of Poly Dimethyl Diallyl Ammonium Chlorides, 20 kilograms of polyoxyethylene nonylphenols more successively and to 4 kilograms of NPs; At the uniform velocity stirred 30 minutes, and made and exempt from the acid-alkali refining agent.
The first gas phase catalyst of in the gas phase catalysis tower, packing into.With waste hydraulic oil after pre-treatment such as dehydration, decon, the mud that deoils, the matter of removing photoresist, deoxidation thing; Pump into header tank, dominant discharge is put into the scission reaction still, and then entering is equipped with in the gas phase catalysis tower of gas phase catalyst; Promptly respectively under the effect of liquid-phase catalyst and gas phase catalyst; At 420～470 ° of C,, approach the crude oil of diesel oil molecules structure with formation with the waste hydraulic oil catalytic pyrolysis.The cracked oil steam that comes out from the gas phase catalysis tower gets into high about 3.5 meters, and in the about 40 centimetres separation column still of diameter, the diesel oil gas that distills out through inner-tower filling material is drawn the back from cat head and got into condensation the condensing surface; After oily water separation, import refining stirred pot, exempt from special use under the effect of acid-alkali refining agent, fully stirred 3～10 minutes; After staticly settling 5～10 minutes; Tell lower floor's residue, the upper strata oil product that obtains obtains refining finished product after filter filters.Product is water white, and clarification is almost tasteless, can be used as oil fuel.Through measuring density 865kg/m
3, kinematic viscosity 7.0mm
2/ s, condensation point-11 ° C, 60 ° of C of close flash point, acidity 5mgKOH/100mL, 1 grade of copper corrosion, No. 2.0, colourity, calorific value>=10800 kcal/kg.
Embodiment 3:
The preparation gas phase catalyst
25 kilograms in the former powder of super-stable Y molecular sieves REUSY, 7 kilograms of high silica ZSM-5 molecular screen primary powders, 10 kilograms of activated aluminas, 65 kilograms in the zeyssatite of the more high silica alumina ratio that will be obtained through dealuminzation by REY type molecular sieve are crossed 120 mesh sieves, mechanical stirring; Mix; Mixed powder and the silica sol binder for preparing are mediated for 18 kilograms, and control pigment mass ratio is 0.55: 1, fully mediates after the extrusion moulding of screw rod banded extruder, pelletizing; Dry under the room temperature; 120 ° of C are down after dry 3 hours, roasting 5 hours under 600 ° of C under oxygen atmosphere, and making diameter is the cylindric gas phase catalyst particle of 4mm.
The preparation liquid-phase catalyst
40 kilograms of cupric oxide, 20 kilograms of pseudo-boehmite dry glue powders and attapulgite are pulverized for 40 kilograms, and mechanical stirring mixes, and crosses 200 mesh sieves, and oven dry is 1 hour under 100 ° of C, makes liquid-phase catalyst.
The acid-alkali refining agent is exempted from preparation
In reaction kettle, add 36 kilograms of diesel oil; Add 7 kilograms of 200 kilograms of triethylene tetramines, 34 kilograms of trolamines, 25 kilograms of Poly Dimethyl Diallyl Ammonium Chlorides, 30 kilograms of polyoxyethylene 20 sorbitan trioleates and n-Heptyl alcohols more successively; At the uniform velocity stirred 30 minutes, and made and exempt from the acid-alkali refining agent.
The first gas phase catalyst of in the gas phase catalysis tower, packing into.With coal tar after pre-treatment such as dehydration, decon, the mud that deoils, the matter of removing photoresist, deoxidation thing; Pump into header tank, dominant discharge is put into the scission reaction still, and then entering is equipped with in the gas phase catalysis tower of gas phase catalyst; Promptly respectively under the effect of liquid-phase catalyst and gas phase catalyst; At 350～400 ° of C,, approach the crude oil of diesel oil molecules structure with formation with the coal tar catalytic pyrolysis.The cracked oil steam that comes out from the gas phase catalysis tower gets into high about 3.5 meters, and in the about 40 centimetres separation column still of diameter, the diesel oil gas that distills out through inner-tower filling material is drawn the back from cat head and got into condensation the condensing surface; After oily water separation, import refining stirred pot, exempt from special use under the effect of acid-alkali refining agent, fully stirred 3～10 minutes; After staticly settling 5～10 minutes; Tell lower floor's residue, the upper strata oil product that obtains obtains refining finished product after filter filters.It is faint yellow that product is, clarification, and free from extraneous odour can be used as oil fuel.Through measuring density 860kg/m
3, kinematic viscosity 6.5mm
2/ s, condensation point-15 ° C, 55 ° of C of close flash point, acidity 5mgKOH/100mL, 1 grade of copper corrosion, No. 2.5, colourity, calorific value>=10200 kcal/kg.
Embodiment 4:
The preparation gas phase catalyst
To cross 120 mesh sieves, mechanical stirring with 26 kilograms in the former powder of rare earth ion metathetical Y zeolite REY, 10 kilograms of high silica ZSM-5 molecular screen primary powders, 12 kilograms of activated aluminas, 55 kilograms of attapulgites; Mix; Mixed powder and the sial complex sol sticker for preparing are mediated for 15 kilograms, and control pigment mass ratio is 0.6: 1, fully mediates after the extrusion moulding of screw rod banded extruder, pelletizing; Dry under the room temperature; 120 ° of C are down after dry 3 hours, roasting 5 hours under 600 ° of C under oxygen atmosphere, and making diameter is the cylindric gas phase catalyst particle of 4mm.
The preparation liquid-phase catalyst
25 kilograms of silicon oxide, 25 kilograms of silico-aluminates and atlapulgite are pulverized for 50 kilograms, and mechanical stirring mixes, and crosses 200 mesh sieves, and oven dry is 1 hour under 100 ° of C, makes liquid-phase catalyst.
The acid-alkali refining agent is exempted from preparation
In reaction kettle, add 33 kilograms of diesel oil; Add 5 kilograms of 280 kilograms of hexahydroaniline, 20 kilograms of N-phenyldiethanol-amines, 22 kilograms of the soaps of cationic polymers, 28 kilograms of polyoxyethylene-type nonionogenic tensides and sec-n-octyl alcohols more successively; At the uniform velocity stirred 30 minutes, and made and exempt from the acid-alkali refining agent.
The first gas phase catalyst of in the gas phase catalysis tower, packing into.With the mixture (about 90: 10 of ratio) of useless gear oil and sewer oil after pre-treatment such as dehydration, decon, the mud that deoils, the matter of removing photoresist, deoxidation thing; Pump into header tank, dominant discharge is put into the scission reaction still, and then entering is equipped with in the gas phase catalysis tower of gas phase catalyst; Promptly respectively under the effect of liquid-phase catalyst and gas phase catalyst; At 430～480 ° of C,, approach the crude oil of diesel oil molecules structure with formation with the mixture through catalytic cracking of useless gear oil and sewer oil.The cracked oil steam that comes out from the gas phase catalysis tower gets into high about 3.5 meters, and in the about 40 centimetres separation column still of diameter, the diesel oil gas that distills out through inner-tower filling material is drawn the back from cat head and got into condensation the condensing surface; After oily water separation, import refining stirred pot, exempt from special use under the effect of acid-alkali refining agent, fully stirred 3～10 minutes; After staticly settling 5～10 minutes; Tell lower floor's residue, the upper strata oil product that obtains obtains refining finished product after filter filters.It is faint yellow that product is, clarification, and free from extraneous odour can be used as oil fuel.Through measuring density 873kg/m
3, kinematic viscosity 7.0mm
2/ s, condensation point-10 ° C, 60 ° of C of close flash point, acidity 6mgKOH/100mL, 1 grade of copper corrosion, No. 3.0, colourity, calorific value>=10600 kcal/kg.
Although relate to a kind of automatic continuous production equipment that splits method waste oil regeneration diesel oil of urging and carried out special description disclosed with reference to embodiment; But the embodiment of above description is illustrative rather than restrictive; Promptly the invention is not restricted to above-mentioned specific embodiment; Under the situation that does not break away from the spirit and scope of the present invention, all variations and modification are all within scope of the present invention.
Claims (10)
1. urge the automatic continuous production technology of splitting method waste oil regeneration diesel oil for one kind, it is characterized in that: comprise following process step: 1) waste oil is carried out pre-treatment; 2) pretreated waste oil is carried out thermo-cracking and catalytic pyrolysis obtains crude oil, wherein catalytic pyrolysis comprises liquid-phase catalysis and gas phase catalysis; 3) crude oil is carried out fractionation; 4) obtain finished product through refining, filtration at last.
2. the automatic continuous production technology of splitting method waste oil regeneration diesel oil of urging according to claim 1, it is characterized in that: said waste oil comprises MO, oils waste oil or the mixture of the two.
3. the automatic continuous production technology of splitting method waste oil regeneration diesel oil of urging according to claim 1 and 2 is characterized in that: said waste oil comprises that used oil, waste lubricating oil, useless gear oil, useless machinery oil, waste hydraulic oil, useless transformer oil, damaged tire are slightly refined oil, slightly oil refining of plastic waste, heavy oil, wax oil, residual oil, coal tar, washing oil, waste cooking oil, acidifying oil, oil-fat plant tankage, useless one or more mixture of deceiving vegetable and animals oils.
4. the automatic continuous production technology of splitting method waste oil regeneration diesel oil of urging according to claim 1 is characterized in that: pre-treatment is dehydration, decon, the mud that deoils, the matter of removing photoresist, the combination of one or more of deoxidation thing in the said step 1).
5. the automatic continuous production technology of splitting method waste oil regeneration diesel oil of urging according to claim 1; It is characterized in that: said step 2) for pretreated waste oil is pumped into header tank; Dominant discharge gets in scission reaction still and the gas phase catalytic tower successively, respectively under the effect of liquid-phase catalyst, gas phase catalyst, at 350～550 ° of C; With the waste oil catalytic pyrolysis, obtain approaching the crude oil of diesel oil molecules structure.
6. the automatic continuous production technology of splitting method waste oil regeneration diesel oil of urging according to claim 5; It is characterized in that: said liquid-phase catalyst is made up of base catalyst, co-catalyst and collaborative regulator; Wherein base catalyst accounts for 10～50% in catalyzer; Co-catalyst accounts for 10～40%, and collaborative regulator accounts for 10～50%, and above per-cent all is weight percentage; Wherein, said base catalyst is one or more the mixture in Aluminum chloride anhydrous, iron(ic)chloride, cupric oxide, aluminum oxide, silicon oxide, Manganse Dioxide, the ZIRCONIUM DIOXIDE 99.5; Said co-catalyst is one or more the mixture in activated alumina, pseudo-boehmite dry glue powder, active silicic acid aluminium, silico-aluminate, sial dry glue powder, macroporous silica gel, the large pore molecular sieve; Said collaborative regulator is one or more the mixture in wilkinite, atlapulgite, zeyssatite, attapulgite, the kaolin.
7. according to claim 5 or the 6 described automatic continuous production technologies of splitting method waste oil regeneration diesel oil of urging; It is characterized in that: said gas phase catalyst comprises following component: Y zeolite, high silica ZSM-5 molecular sieve, activated alumina, carrier and sticker; Said gas phase catalyst active ingredient is a Y zeolite, or the mixture of Y zeolite and high silica ZSM-5 molecular sieve, and said gas phase catalyst staple has silico-aluminate that silicon oxide, aluminum oxide form and rare earth, hydrogen, phosphorus; Wherein Y zeolite accounts for 10～50% in catalyzer; The high silica ZSM-5 molecular sieve accounts for 0～20%, and activated alumina accounts for 10～40%, and carrier accounts for 30～70%; Sticker accounts for 10～20%, and above per-cent all is weight percentage.
8. the automatic continuous production technology of splitting method waste oil regeneration diesel oil of urging according to claim 1; It is characterized in that: treating process adopts and to exempt from the acid-alkali refining agent in the said step 4), and said to exempt from the acid-alkali refining agent be a kind of compound finishing agent, comprises following component: absorption-sinking agent 10～80%; Help active ingredient 5～10%; Cats product 0～10%, nonionogenic tenside 0～10%, cosurfactant 0～5%; Surplus is a diesel oil; Above per-cent all is weight percentage, and wherein, said absorption-sinking agent is one or more the mixture in quadrol, triethylamine, N-alkyl diethylolamine, hexahydroaniline, diethylenetriamine, triethylene diamine, triethylene tetramine, the TEPA; The said active ingredient that helps is one or more the mixture in the carbonic ether of thanomin, trolamine, isopropylamine, N-phenyldiethanol-amine, sulfuric acid vinyl ester, guanidine class; Said cats product is one or more the mixture in the soap, alkyl quaternary ammonium salt, Poly Dimethyl Diallyl Ammonium Chloride, polymethyl acyl-oxygen ethyl-trimethyl salmiac of cationic polymers; Said nonionogenic tenside is one or more the mixture in the tensio-active agent, polyoxyethylene 20 sorbitan monooleate, polyoxyethylene 20 sorbitan trioleate, polyoxyethylene-type nonionogenic tenside, polyoxyethylene nonylphenol nonionogenic tenside of polyoxyethylene sorbitan oleic acid ester class; Said cosurfactant is XU 61518.10, to one or more the mixture in NP, n-Heptyl alcohol, n-Octanol, the sec-n-octyl alcohol.
9. the automatic continuous production technology of splitting method waste oil regeneration diesel oil of urging according to claim 1 is characterized in that: this technology also comprises waste gas recovery burning, and the flue gas heat recovering step.
10. the automatic continuous production technology of splitting method waste oil regeneration diesel oil of urging according to claim 1, it is characterized in that: whole process flow is the process in the automatic continuous production of enclosed space charging and deslagging.
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