CN114634826B - Method and system for preparing jet fuel, white oil and lubricating oil base oil by hydrogenating waste oil - Google Patents
Method and system for preparing jet fuel, white oil and lubricating oil base oil by hydrogenating waste oil Download PDFInfo
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- 239000002699 waste material Substances 0.000 title claims abstract description 103
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- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 91
- 239000000047 product Substances 0.000 claims abstract description 58
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
- C10G67/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/10—Lubricating oil
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/14—White oil, eating oil
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a method and a system for preparing jet fuel, white oil and lubricating oil base oil by hydrogenating waste oil, wherein waste coal tar, rubber oil, waste mineral oil and waste biomass oil are mixed according to a certain proportion, the mixed waste oil sequentially passes through the working procedures of pretreatment, suspension bed hydrogenation, fixed bed segmented time-sharing hydrogenation, fractionation and the like, the comprehensive and effective reuse of various dangerous waste oil products is realized, and the preparation of high-value jet fuel, industrial white oil, lubricating oil base oil products and the like can be realized by adjusting the proportion of 4 kinds of dangerous waste oil products; oil-soluble molybdenum isooctanoate is selected as a suspension bed hydrogenation catalyst, and the molybdenum isooctanoate is decomposed into a nano molybdenum sulfide catalyst in situ, is highly dispersed in an oil phase and has high reaction activity; the fixed bed sectional time-sharing hydrogenation effectively avoids the problems of aggravation of final product weight and reduction of effective components caused by high reaction temperature in full fraction processing.
Description
Technical Field
The invention belongs to the technical field of deep processing of hazardous waste oil products, and particularly relates to a method and a system for preparing jet fuel, white oil and lubricating oil base oil by hydrogenating waste oil.
Background
Climate change is a global problem facing human beings, and greenhouse gases are increased rapidly with the increase of carbon dioxide emission in various countries, thus forming a threat to life systems. Under the background, the carbon peak-to-peak and carbon neutralization targets are formally proposed in China, and how to achieve the double-carbon target while increasing energy supply is the primary problem of the energy industry in view of the carbon dioxide emission reduction target with a huge base number. The hazardous waste resources are reasonably utilized, the available components in hazardous waste oil products (waste coal tar, rubber oil, waste biomass oil and waste mineral oil) are recycled to the maximum extent, and the change of waste into valuable is one of effective means for solving the problem.
The waste coal tar is obtained by simply recovering and treating slag-containing, water-containing and mud-containing waste materials generated in the coal tar purification process, wherein the water content, the solid content and the asphaltene heavy component content are all higher than those of normal coal tar, the conventional fixed bed process cannot be used for carrying out hydrogenation treatment, the molecular structure of the waste coal tar is complex, the waste coal tar mainly contains polycyclic aromatic hydrocarbons such as naphthalene and anthracene, aromatic oxygen-containing compounds, heterocyclic compounds containing nitrogen and sulfur and other various organic matters, and the waste coal tar has serious environmental hazard and carcinogenicity of human bodies. Rubber is widely applied to the national economy field, rubber products such as used waste tires and the like are increased year by year, and a technology for cracking the waste rubber products into fuel oil products already exists. However, because of the existence of a large amount of fused ring aromatic compounds and various additive residues in the rubber pyrolysis oil product, if the rubber pyrolysis oil product cannot be cleanly treated, the special foul smell and the harmfulness of the fused ring aromatic hydrocarbon become main problems for limiting the high-quality utilization. The waste organic residue represented by waste biomass oil and the like contains a large amount of compounds such as fatty acid, fatty acid ester and the like, and the utilization value of the waste organic residue can be obviously improved by removing the oxygen-containing compounds in the waste organic residue through a reasonable hydro-conversion scheme. The waste lubricating oil resources contain a large amount of additives and metal impurities, hydrocarbon molecules are subjected to oxidation, fracture, polycondensation and other reactions in a high-temperature shearing environment, and the requirements for lubrication are difficult to meet after the hydrocarbon molecules are deteriorated.
The waste coal tar is mainly composed of aromatic hydrocarbon, and heteroatoms such as nitrogen and oxygen are mostly present in polycyclic aromatic hydrocarbon; the rubber oil mainly comprises aromatic hydrocarbon and naphthenic hydrocarbon compounds, and a large amount of rubber reinforcing additives and auxiliary agent components are carried in the oil product; organic residues such as vegetable oils are mainly compounds such as fatty acids and fatty acid esters; the waste lubricating oil contains paraffin as main component and also contains great amount of inorganic matter or metal impurity. The traditional processing scheme can not carry out unified treatment on the waste oil products with various components, the balance and the availability of the product performance are poor due to the fact that the components of the product are single relatively after the single-component deep processing, and meanwhile, the traditional processing technology has the problems of low utilization rate and the like.
The patent with the application number of 202010866073.4 discloses a method for producing aviation kerosene and biomass oil and coal tar jointly, the method comprises the steps of firstly separating the coal tar into a light fraction and a heavy fraction, then mixing the separated light fraction and the biomass oil in proportion, converting the raw materials into products meeting the requirements of No. 3 aviation kerosene in a mode of combining hydrofining and hydroisomerization, and using a fixed bed reactor in the hydrogenation process. Although the method can achieve the purpose of preparing aviation kerosene, the method has a plurality of problems in the aspect of effective utilization of resources, on one hand, the method only utilizes lighter fractions in coal tar, the effective utilization rate of the coal tar is not more than 70%, heavy components left by fractionation are more difficult to treat, and still serious environmental pollution is caused; on the other hand, the aviation kerosene processed by adopting the technical route can only meet the requirement of No. 3 aviation kerosene, and can not meet the requirement of preparing high-flash-point jet fuel in the aspects of density, distillation range, flash point and the like.
The patent with the application number of 202010942603.9 discloses a method and a system for preparing gasoline and diesel oil by mixing and hydrogenating coal tar and biomass oil. Although the technology can realize the purpose of preparing the fuel oil by mixing the coal tar and the biomass oil, the three-stage hydrofining can not realize the preparation of the jet fuel with low freezing point and high flash point and the base oil, and the technical route is difficult to convert the heavy components in the coal tar at more than 360 ℃.
The patent with the application number of 201710694332.8 discloses a regeneration process for producing low-freezing base oil by a waste lubricating oil hydrogen-all method. Although the waste lubricating oil is processed into the low-freezing base oil through the steps of atmospheric and vacuum fractionation, propane refining, hydrofining, hydroisomerization and the like, the method uses a two-stage fixed bed hydrogenation process, and the hydrogenation product completely depends on the raw material waste lubricating oil and cannot meet the requirements for processing raw materials such as waste coal tar, rubber oil, waste biomass oil and the like.
The patent with the application number of 201610827700.7 discloses a method for the hydrogenation and regeneration utilization of a wide fraction of a waste lubricating oil. The process comprises the steps of performing hydrocracking and electric desalting impurity removal on waste lubricating oil in a suspension bed in the presence of an oil-soluble catalyst, performing hydro-upgrading, hydro-refining and cut-cutting on pretreated full distillate oil to obtain diesel oil and a regenerated base oil product, wherein the suspension bed hydrogenation uses an oil-soluble substance synthesized from hexadecyl trimethyl ammonium hydroxide and tetrathio ammonium molybdate as the catalyst. Although the method can realize the regeneration of the waste lubricating oil, the method cannot realize the processing of the hazardous waste oil products which are rich in polycyclic aromatic hydrocarbons or fatty acids such as coal tar, rubber oil and waste biomass oil; ammonium compounds are used as the precursor of the suspension bed hydrogenation catalyst, ammonia gas can be released in the in-situ decomposition and vulcanization process in a hydrogen environment, and the hydrogenation and denitrification reaction of the high-nitrogen-content raw material is not facilitated; the oil product after the suspension bed hydrogenation is sent into a subsequent fixed bed in a full fraction mode to carry out deep hydrogenation reaction, in order to meet the hydrogenation depth of heavy fraction, the oil product is inevitably cracked in a reactor, the yield of the base oil fraction is low, and the production of high-end fuel oil products such as jet fuel and the like cannot be realized.
Therefore, the development of a method which has lower investment and operation cost and can prepare products such as jet fuel, white oil, lubricating oil base oil and the like by processing and reasonably blending the waste oil mixture without the limitation of raw materials is of great significance.
Disclosure of Invention
In order to overcome the defects of the method, the invention provides a method for preparing jet fuel, white oil and lubricating oil base oil by taking mixed hazardous waste oil products such as waste coal tar, rubber oil, waste mineral oil, waste biomass oil and the like which are adjusted according to the proportion as raw materials and adopting a mode of coupling suspension bed hydrogenation and fixed bed hydrogenation.
Meanwhile, the invention also provides a system for preparing jet fuel, white oil and lubricating oil base oil by hydrogenating the waste oil.
The method for preparing jet fuel, white oil and lubricating oil base oil by hydrogenating waste oil, which is adopted for solving the technical problems, comprises the following steps of:
step 1: waste oil mixing and pretreatment
According to the mass percentage, 5 to 85 percent of waste coal tar, 5 to 80 percent of rubber oil, 5 to 85 percent of waste mineral oil and 5 to 85 percent of waste biomass oil are mixed evenly in a component adjusting mixer to obtain mixed waste oil; removing most of solid or insoluble impurities and water from the mixed waste oil by a centrifugal machine, heating the mixed waste oil to 100-150 ℃ in a heater, mixing the waste oil with a dehydration and desalination auxiliary agent, then feeding the mixture into a dehydration tank, maintaining the pressure in the dehydration tank to be 0.5-1.5 MPa, completing demulsification and dehydration of the mixed waste oil, feeding the dehydrated mixed waste oil into a flash evaporation dehydration tower for deep dehydration, and removing free water, emulsified water and salt in an oil phase.
Step 2: hydrogenation in suspension bed
Adding an oil-soluble catalyst precursor and a vulcanizing agent into the deeply dehydrated mixed waste oil, mixing the deeply dehydrated mixed waste oil with hydrogen after being boosted by a high-pressure feed pump, feeding the mixture into a first heating furnace, heating the mixture by the first heating furnace, feeding the mixture into a suspension bed reactor, carrying out hydrogenation reaction on the mixture in the suspension bed reactor to remove metal and carbon residue, and removing part of sulfur, nitrogen and oxygen, so that the metal removal rate, the carbon residue removal rate and the sulfide removal rate in the mixed waste oil are respectively greater than 95%, greater than 94% and greater than 70%; separating the hydrogenation product of the suspension bed into a gas phase and a liquid phase through a first high-pressure separator, allowing the gas phase to enter a first cold low-pressure separator for further separation into hydrogen and naphtha, allowing the liquid phase to enter a first hot low-pressure separator for further separation into naphtha and pre-hydrogenated distillate oil, and allowing the pre-hydrogenated distillate oil to enter a first fractionating tower for atmospheric and vacuum fractionation into naphtha, a fuel oil fraction at 180-320 ℃, a base oil fraction at 320-480 ℃ and bottom reducing oil; the hydrogen separated by the first cold low-pressure separator is recycled after being boosted by a recycle hydrogen compressor, naphtha separated by the first cold low-pressure separator and the first hot low-pressure separator and naphtha fractionated by the first fractionating tower are output as products, the fuel oil fraction and the base oil fraction respectively enter a fuel oil fraction storage tank and a base oil fraction storage tank, the catalyst component mixed in the bottom-reducing oil and the bottom-reducing oil is boosted by a bottom-reducing oil circulating pump and then sent back to the suspended bed reactor, and the suspended bed hydrogenation reaction is continuously carried out. Wherein the oil-soluble catalyst precursor is oil-soluble molybdenum isooctanoate.
And 3, step 3: fixed bed hydrogenation
Mixing the fuel oil fraction in a fuel oil fraction storage tank and the base oil fraction in a base oil fraction storage tank with a vulcanizing agent and hydrogen respectively in an alternate feeding mode, then, heating the mixture in a second heating furnace, then, sending the mixture into a first refining reactor, carrying out deep hydrofining reaction in the first refining reactor, removing sulfur, nitrogen and aromatic hydrocarbon components, mixing a hydrofining product with the hydrogen, sending the mixture to an isomerization reactor, carrying out isomerization reaction in the isomerization reactor, carrying out heat exchange on the reacted oil through a heat exchanger, then, sending the reacted oil into a stripping tower, finishing stripping of hydrogen sulfide and ammonia components dissolved in the oil in the stripping tower, sending the stripped oil and new hydrogen to a second refining reactor after mixing, carrying out deep hydrogenation saturation reaction in the second refining reactor, removing olefin and aromatic hydrocarbon components, sending the gas phase into a second high-pressure separator for gas-liquid separation after the reaction is finished, sending the gas phase into a second cold low-pressure separator for further separation into naphtha and hydrogen gas, and sending the liquid phase into a second hot low-pressure separator for further separation into distillate oil and hydrogenation modification; naphtha separated by the second cold low-pressure separator and the second hot low-pressure separator is output as a product, hydrogen separated by the second cold low-pressure separator is boosted by a circulating hydrogen compressor and then sent to a stripping tower to be used as stripping gas for recycling, the content of sulfur and nitrogen in oil stripped by the stripping tower is ensured to be less than 5ppm, and hydrogenated modified distillate oil separated by the second hot low-pressure separator is sent to a second fractionating tower to be fractionated into naphtha, jet fuel, white oil, lubricating oil base oil and rubber plasticizer naphthenic base mineral oil products.
In the step 1, when the total mass percentage of the waste coal tar and the rubber oil accounts for 10-50% of the mixed waste oil, the products fractionated by the second fractionating tower in the step 3 mainly comprise naphtha, biological aviation kerosene, industrial white oil and lubricating oil base oil; in the step 1, when the total mass percentage of the waste coal tar and the rubber oil accounts for 60-90% of the mixed waste oil, the products fractionated by the second fractionating tower in the step 3 mainly comprise high-flash-point jet fuel, industrial white oil and rubber plasticizer naphthenic mineral oil.
In the step 1, the injection amount of the dehydration and desalination auxiliary agent is 100 to 1000ppm.
In the step 2, the injection amount of the oil-soluble molybdenum isooctanoate is 100 ppm-1000 ppm, and the oil-soluble molybdenum isooctanoate is decomposed and sulfurized into a nano-scale molybdenum sulfide catalyst in situ in a hydrogen environment and is highly dispersed in an oil phase.
In the step 2, the hydrogenation reaction temperature of the suspension bed is 360-450 ℃, the reaction pressure is 12-18 MPa, and the volume airspeed is 0.5-1.3 h -1 The volume ratio of hydrogen to oil is 800-1500.
In the above step 2 and step 3, the amount of the vulcanizing agent to be injected is 100 to 500ppm. The vulcanizing agents are common vulcanizing agents such as carbon disulfide, dimethyl disulfide, liquid sulfur and the like.
In the step 3, when the fixed bed hydrogenation is carried out on the fuel oil fraction, the deep hydrogenation refining reaction temperature is 300-360 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 1000-1500, and the volume space velocity is 0.4-0.7 h -1 (ii) a The isomerization reaction temperature is 320-350 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 1000-2000 -1 (ii) a The deep hydrogenation saturation reaction temperature is 150-200 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 500-1000 -1 。
In the step 3, when the base oil fraction is subjected to fixed bed hydrogenation, the deep hydrofining reaction temperature is 360-400 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 1200-2000, and the volume space velocity is 0.4-0.7 h -1 (ii) a The isomerization reaction temperature is 350-400 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 1000-2000 -1 (ii) a The deep hydrogenation saturation reaction temperature is 200-250 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 500-1000 -1 。
In the step 3, the catalyst for the deep hydrorefining reaction adopts a bimodal distribution of pore diametersThe phosphorus modified alumina is used as a carrier, niO 2-3 percent and MoO are loaded 3 5％～8％、WO 3 18 to 25 percent; the catalyst for isomerization reaction takes silicon modified ZSM-5 as a carrier, and NiO is loaded by 1.5-5 percent; the catalyst for the deep hydrogenation saturation reaction takes amorphous silicon-aluminum as a carrier, and loads NiO with the content of 8-15 percent; wherein the loading amount of the active component is calculated by taking the mass of the catalyst as 100%.
The system for preparing jet fuel, white oil and lubricating oil base oil by hydrogenating the waste oil comprises the following steps: the device comprises a raw material pretreatment unit, a suspension bed hydrogenation unit and a fixed bed hydrogenation unit; wherein, the raw material pretreatment unit consists of a component adjusting mixer, a centrifuge, a heater, a dehydration tank and a flash evaporation dehydration tower; the suspension bed hydrogenation unit is formed by connecting a high-pressure feed pump, a first heating furnace, a suspension bed reactor, a first high-pressure separator, a first cold low-pressure separator, a first hot low-pressure separator, a first fractionating tower, a bottom-reducing oil circulating pump, a fuel oil fraction storage tank and a base oil fraction storage tank; the fixed bed hydrogenation unit is formed by connecting a second heating furnace, a first refining reactor, an isomerization reactor, a heat exchanger, a stripping tower, a second refining reactor, a second high-pressure separator, a second cold low-pressure separator, a second hot low-pressure separator and a second fractionating tower. The waste coal tar, the rubber oil, the waste biomass oil and the waste mineral oil pipeline are respectively communicated with a component adjusting mixer, and an outlet of the component adjusting mixer is sequentially communicated with a centrifugal machine, a heater, a dehydration tank and a flash evaporation dehydration tower; the bottom outlet of the flash dehydration tower is connected with the inlet of a high-pressure feed pump, the outlet of the high-pressure feed pump is connected with a circulating hydrogen pipeline at the top outlet of a first cold low-pressure separator and a new hydrogen pipeline after being converged and then connected with the feed inlet of a first heating furnace, the discharge outlet of the first heating furnace is communicated with the outlet pipeline of a bottom reducing oil circulating pump after being converged and then communicated with the bottom inlet of a suspended bed reactor, the top outlet of the suspended bed reactor is communicated with a first high-pressure separator, the top outlet of the first high-pressure separator is communicated with a first cold low-pressure separator, the bottom outlet of the first high-pressure separator is communicated with a first hot low-pressure separator, the bottom outlet of the first cold low-pressure separator and the top outlet of the first hot low-pressure separator are both connected with a naphtha output pipeline, the bottom outlet of the first hot low-pressure separator is communicated with a first stripping tower, the first stripping tower is connected with the inlet of the bottom reducing oil circulating pump, the upper fuel oil outlet in the first stripping tower is communicated with a fuel oil fraction storage tank, the lower portion in the first stripping tower is connected with a base oil fraction storage tank, and the fuel oil fraction storage tank and the base oil storage tank are respectively communicated with the new hydrogen pipeline and the top outlet circulating hydrogen pipeline and then communicated with the feed inlet of a second heating furnace; the second heating furnace discharge port is communicated with the first refining reactor top inlet, the first refining reactor bottom outlet is communicated with the heterogeneous reactor top inlet after being converged with a fresh hydrogen pipeline and a stripping tower top outlet circulating hydrogen pipeline, the heterogeneous reactor bottom outlet is communicated with the stripping tower middle inlet through a heat exchanger, the stripping tower bottom outlet is communicated with the second refining reactor top inlet after being converged with the fresh hydrogen pipeline, the second refining reactor bottom outlet is communicated with the second high-pressure separator, the second high-pressure separator top outlet is communicated with the second cold low-pressure separator, the second high-pressure separator bottom outlet is communicated with the second hot low-pressure separator, the second hot low-pressure separator bottom outlet is communicated with the second fractionating tower lower part, and the second cold low-pressure separator bottom outlet and the second hot low-pressure separator top outlet are both connected with a naphtha output pipeline.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention provides a system and a method for treating waste coal tar, rubber oil, waste mineral oil and waste biomass oil in a unified and high-valued manner, which firstly provide that the waste coal tar, the rubber oil, the waste mineral oil and the waste biomass oil are mixed according to a certain proportion, the mixed waste oil sequentially passes through the working procedures of pretreatment, suspension bed hydrogenation, fixed bed hydrogenation, fractionation and the like, the effective reuse of various dangerous waste oil products is realized, and the preparation of high-value jet fuel, industrial white oil, lubricating oil base oil products and the like can be realized by adjusting the proportion of 4 dangerous waste oil products.
2. In the method, the mixed waste oil of the waste coal tar, the rubber oil, the waste mineral oil and the waste biomass oil is used for processing and preparing the high-flash-point jet fuel for the first time.
3. The invention provides a system and a method for hydrogenation of a suspension bed coupling fixed bed, and in the system and the method, oil generated by hydrogenation of the suspension bed is fractionated into different functional fractions, and the different functional fractions enter the fixed bed for processing in an alternative (segmented time-sharing) feeding mode, so that the problems of aggravation of the final product in light weight and reduction of effective components caused by high reaction temperature in the whole fraction processing are effectively avoided.
4. In the method, oil-soluble molybdenum isooctanoate is selected as a catalyst for hydrogenation of the waste oil suspension bed, the molybdenum isooctanoate can be decomposed into a nano molybdenum sulfide catalyst in situ in a suspension bed reaction system, the nano molybdenum sulfide catalyst is highly dispersed in an oil phase, the reaction activity is high, and the problem of inhibition of hydrodenitrification caused by decomposition of an ammonium-containing catalyst can be effectively avoided by the molybdenum isooctanoate.
5. The method has the advantages that solid impurities, chlorine and other harmful impurities and water in the waste oil are removed through pretreatment, and the process is simple; the suspension bed hydrogenation adopts the oil-soluble catalyst precursor to decompose into a highly dispersed nano-grade molybdenum sulfide active phase in situ, the process can accept wide raw material adjustment range, most metal impurities, colloid and asphaltene in the waste oil can be removed by reaction, and the level of moderation and refining is achieved; the fixed bed hydrogenation adopts a refined catalyst which takes tungsten, nickel and molybdenum as active metals, an isomerization catalyst which takes tungsten, nickel and molybdenum as active metals and a refined catalyst which takes reduced nickel as active metals, and the catalyst does not contain noble metals and has low operation cost.
Drawings
FIG. 1 is a schematic diagram of the process for producing jet fuel, white oil and lubricant base oil by hydrogenating waste oil in example 1.
In the figure: 1-component adjusting mixer, 2-centrifuge, 3-heater, 4-dehydration tank, 5-flash dehydration tower, 6-high pressure feed pump, 7-first heating furnace, 8-suspension bed reactor, 9-first high pressure separator, 10-first cold low pressure separator, 11-first hot low pressure separator, 12-first fractionating tower, 13-bottom oil reducing circulating pump, 14-fuel oil fraction storage tank, 15-base oil fraction storage tank, 16-second heating furnace, 17-first refining reactor, 18-isomerization reactor, 19-heat exchanger, 20-stripping tower, 21-second refining reactor, 22-second high pressure separator, 23-second cold low pressure separator, 24-second hot low pressure separator and 25-second fractionating tower.
Detailed Description
The invention will be described in more detail below with reference to the drawings and examples, but the scope of protection of the invention is not limited to these examples.
As shown in FIG. 1, the system for preparing jet fuel, white oil and lubricant base oil by hydrogenating waste oil in this embodiment mainly comprises a raw material pretreatment unit, a suspended bed hydrogenation unit and a fixed bed hydrogenation unit. Wherein, the raw material pretreatment unit consists of a component adjusting mixer 1, a centrifuge 2, a heater 3, a dehydration tank 4 and a flash evaporation dehydration tower 5; the suspended bed hydrogenation unit is formed by connecting a high-pressure feed pump 6, a first heating furnace 7, a suspended bed reactor 8, a first high-pressure separator 9, a first cold low-pressure separator 10, a first hot low-pressure separator 11, a first fractionating tower 12, a bottom oil reducing circulating pump 13, a fuel oil fraction storage tank 14 and a base oil fraction storage tank 15; the fixed bed hydrogenation unit is formed by connecting a second heating furnace 16, a first refining reactor 17, an isomerization reactor 18, a heat exchanger 19, a stripping tower 20, a second refining reactor 21, a second high-pressure separator 22, a second cold low-pressure separator 23, a second hot low-pressure separator 24 and a second fractionating tower 25.
The waste coal tar, the rubber oil, the waste biomass oil and the waste mineral oil pipeline are respectively communicated with the component adjusting mixer 1, and the outlet of the component adjusting mixer 1 is sequentially communicated with the centrifuge 2, the heater 3, the dehydration tank 4 and the flash dehydration tower 5 through pipelines; the bottom outlet of a flash dehydration tower 5 is connected with the inlet of a high-pressure feed pump 6 through a pipeline, the outlet of the high-pressure feed pump 6 is connected with a circulating hydrogen pipeline at the top outlet of a first cold low-pressure separator 10 and a new hydrogen pipeline through pipelines and then is connected with the feed inlet of a first heating furnace 7, the discharge port of the first heating furnace 7 is connected with the bottom inlet of a suspended bed reactor 8 through a pipeline and a circulating pump 13 for reducing bottom oil through a pipeline and then is communicated with the bottom outlet of the suspended bed reactor 8, the top outlet of the suspended bed reactor 8 is communicated with a first high-pressure separator 9 through a pipeline, the top outlet of the first high-pressure separator 9 is communicated with the first cold low-pressure separator 10 through a pipeline, the bottom outlet of the first hot low-pressure separator 11 is communicated with a naphtha output pipeline through a pipeline, the bottom outlet of the first hot low-pressure separator 11 is communicated with a first fractionating tower 12 through a pipeline, the first fractionating tower 12 is connected with the inlet of the circulating pump 13 for reducing bottom oil through a pipeline, the upper fuel oil outlet in the first fractionating tower 12 is communicated with a fuel oil storage tank 14 through a pipeline, the lower part of the first fractionating tower 12 is communicated with a base oil storage tank 14 and a circulating tank 15, and a new hydrogen storage tank 15 through a pipeline and a new hydrogen storage tank 15; the discharge port of the second heating furnace 16 is communicated with the top inlet of the first refining reactor 17 through a pipeline, the bottom outlet of the first refining reactor 17 is communicated with the top inlet of the isomerization reactor 18 after being converged with a fresh hydrogen pipeline and a circulating hydrogen pipeline at the top outlet of the stripping tower 20 through pipelines, the bottom outlet of the isomerization reactor 18 is communicated with the middle inlet of the stripping tower 20 through a heat exchanger 19 through a pipeline, the bottom outlet of the stripping tower 20 is communicated with the top inlet of the second refining reactor 21 after being converged with the fresh hydrogen pipeline through a pipeline, the bottom outlet of the second refining reactor 21 is communicated with the second high-pressure separator 22 through a pipeline, the top outlet of the second high-pressure separator 22 is communicated with the second cold low-pressure separator 23 through a pipeline, the bottom outlet of the second high-pressure separator 22 is communicated with the second hot low-pressure separator 24 through a pipeline, the bottom outlet of the second cold low-pressure separator 23 and the top outlet of the second hot low-pressure separator 24 are both connected with a naphtha output pipeline.
The method for preparing jet fuel, white oil and lubricating oil base oil by hydrogenating the waste oil by adopting the system comprises the following steps:
step 1: waste oil mixing and pretreatment
According to the mass percentage, 5-85% of waste coal tar, 5-80% of rubber oil, 5-85% of waste mineral oil and 5-85% of waste biomass oil are mixed uniformly in a component adjusting mixer 1 to obtain mixed waste oil; most of solid or insoluble impurities and water in the mixed waste oil are removed by a centrifugal machine 2, then the mixed waste oil is heated to 100-150 ℃ in a heater 3, the mixed waste oil is mixed with a dehydration and desalination auxiliary agent and then enters a dehydration tank 4, the pressure in the dehydration tank 4 is maintained to be 0.5-1.5 MPa, the demulsification and the dehydration of the mixed waste oil are completed, the dehydrated mixed waste oil enters a flash evaporation dehydration tower 5 for deep dehydration, and the free water, the emulsified water and the salt in the oil phase are removed. Wherein, the dehydration desalting auxiliary agent selects ZH-002 type and ZH-004 type auxiliary agents which take polyethers and acidic organic compounds of Heng New materials, inc. in Shaanxi as main components, and the injection amount of the auxiliary agents is 100-1000 ppm.
Step 2: hydrogenation in suspension bed
Adding an oil-soluble catalyst precursor and a vulcanizing agent into the deeply dehydrated mixed waste oil, boosting the pressure by a high-pressure feed pump 6, mixing the mixture with hydrogen, feeding the mixture into a first heating furnace 7, heating the mixture by the first heating furnace 7, feeding the mixture into a suspension bed reactor 8, performing a suspension bed hydrogenation reaction in the suspension bed reactor 8, removing metals and carbon residues, and removing part of sulfur, nitrogen and oxygen, so that the metal removal rate in the mixed waste oil is more than 95%, the carbon residue removal rate is more than 94% and the sulfide removal rate is more than 70%; the hydrogenation product of the suspension bed is separated into a gas phase and a liquid phase through a first high-pressure separator 9, the gas phase flows out from an outlet at the top of the first high-pressure separator 9 and enters a first cold low-pressure separator 10 to be further separated into hydrogen and naphtha, the liquid phase flows out from an outlet at the bottom of the first high-pressure separator 9 and enters a first hot low-pressure separator 11 to be further separated into naphtha and pre-hydrogenated distillate oil, the pre-hydrogenated distillate oil flows out from an outlet at the bottom of the first hot low-pressure separator 11 and enters a first fractionating tower 12 to be fractionated under normal pressure and reduced pressure into naphtha, fuel oil fraction at 180-320 ℃, base oil fraction at 320-480 ℃ and bottom-reduced oil; hydrogen separated by the first cold low-pressure separator 10 flows out from a top outlet, enters a circulating hydrogen pipeline, is subjected to pressure boosting by a circulating hydrogen compressor and is recycled, naphtha separated by the first cold low-pressure separator 10 and the first hot low-pressure separator 11 flows out from the bottom to be output as a product, naphtha fractionated by the first fractionating tower 12 is output as a product, the fuel oil fraction and the base oil fraction respectively enter a fuel oil fraction storage tank 14 and a base oil fraction storage tank 15, and the base oil are reducedThe mixed catalyst components are pressurized by a bottom oil reducing circulating pump 13 and then sent back to the suspension bed reactor 8, and the suspension bed hydrogenation reaction is continuously carried out. Wherein the oil-soluble catalyst precursor is oil-soluble molybdenum isooctanoate which is decomposed and sulfurized into a nano-scale molybdenum sulfide catalyst in situ in a hydrogen environment and is highly dispersed in an oil phase, and the injection amount of the oil-soluble catalyst precursor is 100ppm to 1000ppm; the vulcanizing agents are common vulcanizing agents such as carbon disulfide, dimethyl disulfide, liquid sulfur and the like, and the injection amount of the vulcanizing agents is 100-500 ppm; the hydrogenation reaction temperature of the suspension bed is 360-450 ℃, the reaction pressure is 12-18 MPa, and the volume airspeed is 0.5-1.3 h -1 The volume ratio of hydrogen to oil is 800-1500.
And step 3: fixed bed hydrogenation
Mixing the fuel oil fraction in the fuel oil fraction storage tank 14 and the base oil fraction in the base oil fraction storage tank 15 with a vulcanizing agent and hydrogen respectively in an alternate feeding mode, then feeding the mixture into a second heating furnace 16 for heating, then feeding the mixture into a first refining reactor 17, carrying out deep hydrofining reaction in the first refining reactor 17 to remove components such as sulfur, nitrogen and aromatic hydrocarbon, enabling a hydrofining product to flow out from a bottom outlet of the first refining reactor 17 to be mixed with the hydrogen and then to be fed into a top inlet of an isomerization reactor 18, carrying out isomerization reaction in the isomerization reactor 18, enabling an oil product after reaction to flow out from a bottom outlet of the isomerization reactor 18 to enter a middle inlet of a stripping tower 20 after heat exchange by a heat exchanger 19, and finishing stripping of components such as hydrogen sulfide and ammonia dissolved in the stripping tower 20, the stripped oil product flows out from the bottom outlet of the stripping tower 20 and is mixed with new hydrogen and then is sent to the top inlet of the second refining reactor 21, deep hydrogenation saturation reaction is carried out in the second refining reactor 21 to remove components which are not beneficial to product performance, such as olefin, aromatic hydrocarbon and the like, the reaction product flows out from the bottom outlet of the second refining reactor 21 and enters the second high-pressure separator 22 for gas-liquid separation, the gas phase flows out from the top outlet of the second high-pressure separator 22 and enters the second cold low-pressure separator 23 for further separation into naphtha and hydrogen, and the liquid phase flows out from the bottom outlet of the second high-pressure separator 22 and enters the second hot low-pressure separator 24 for further separation into naphtha and hydrogenation modified distillate oil; naphtha separated by the second cold low-pressure separator 23 flows out from a bottom outlet and is output as a product, naphtha separated by the second hot low-pressure separator 24 flows out from a top outlet and is also output as a product, hydrogen separated by the second cold low-pressure separator 23 flows out from the top outlet, is boosted by a recycle hydrogen compressor and is sent to the stripping tower 20 to be recycled as stripping gas, and the content of sulfur and nitrogen in oil stripped by the stripping tower 20 is ensured to be less than 5ppm; the hydroupgrading distillate oil separated by the second hot low pressure separator 24 flows out from the bottom outlet and enters a second fractionating tower 25 for fractionation to obtain naphtha, jet fuel, white oil, lubricating oil base oil and rubber plasticizer naphthenic mineral oil products.
In the step 3, when the fixed bed hydrogenation is carried out on the fuel oil fraction, the deep hydrogenation refining reaction temperature is 300-360 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 1000-1500, and the volume space velocity is 0.4-0.7 h -1 (ii) a The isomerization reaction temperature is 320-350 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 1000-2000 -1 (ii) a The deep hydrogenation saturation reaction temperature is 150-200 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 500-1000 -1 . When the base oil fraction is hydrogenated by a fixed bed, the deep hydrofining reaction temperature is 360-400 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 1200-2000, and the volume space velocity is 0.4-0.7 h -1 (ii) a The isomerization reaction temperature is 350-400 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 1000-2000, the volume space velocity is 0.5-1.5 h -1 (ii) a The deep hydrogenation saturation reaction temperature is 200-250 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 500-1000, and the volume space velocity is 0.5-4 h -1 . The catalyst for the deep hydrorefining reaction adopts phosphorus modified alumina with bimodal distribution of pore diameter as a carrier, and NiO 2-3% and MoO are loaded 3 5％～8％、WO 3 18 to 25 percent; the catalyst for the isomerization reaction takes silicon modified ZSM-5 as a carrier and loads NiO by 1.5 to 5 percent; the catalyst for the deep hydrogenation saturation reaction takes amorphous silicon-aluminum as a carrier and loads 8 to 15 percent of NiO, wherein the loading amount of active components is calculated by taking the mass of the catalyst as 100 percent.
In the step 3, when the total mass percent of the waste coal tar and the rubber oil used in the step 1 accounts for 10-50% of the mixed waste oil, the products fractionated by the second fractionating tower 25 mainly comprise naphtha, biological aviation kerosene, industrial white oil and lubricating oil base oil; when the total mass percentage of the waste coal tar and the rubber oil used in the step 1 accounts for 60-90% of the mixed waste oil, the products fractionated by the second fractionating tower 25 in the step 3 mainly comprise high flash point jet fuel, industrial white oil and rubber plasticizer naphthenic base mineral oil.
Jet fuel, industrial white oil, lubricating oil base oil and rubber plasticizer naphthenic mineral oil are produced by using the waste coal tar with physicochemical properties shown in Table 1, the rubber oil with physicochemical properties shown in Table 2, the waste mineral oil with physicochemical properties shown in Table 3 and the waste biomass oil with physicochemical properties shown in Table 4 as raw materials according to the mass percentage distribution ratios of examples 1 to 3 shown in Table 5, the dehydration tank operation conditions shown in Table 6, the suspension bed hydrogenation reaction conditions shown in Table 7 and the fixed bed hydrogenation reaction conditions shown in Table 9, wherein the hydrogenation results of the suspension bed are shown in Table 8, and the hydrogenation results of the fixed bed are shown in tables 10 to 19.
TABLE 1 physical and chemical properties of waste coal tar
TABLE 2 rubber oil physico-chemical Properties
TABLE 3 physicochemical Properties of waste mineral oils
TABLE 4 physical and chemical Properties of waste Biomass oil
| Item | Data of |
| Density (20 ℃ C.), g/cm 3 | 0.910 |
| Kinematic viscosity (40 ℃ C.), mm 2 /s | 32.15 |
| Pour point, |
25 |
| Water fraction volatile matter content + insoluble impurity content (mass fraction)% | 1.35 |
| pH value | 6.7 |
| Saponification number (calculated as KOH), mg/kg | 188 |
| Phospholipid content (mass fraction)% | 0.2 |
| Content (mass fraction) of unsaponifiable matter | 0.4 |
| Content (mass fraction) of esterified substance% | 97 |
TABLE 5 raw material mixing ratio and macroscopic Properties
TABLE 6 operating conditions of the dehydration tank
| Item | Example 1 | Example 2 | Example 3 |
| Auxiliary agent | ZH-002 | ZH-002 | ZH-004 |
| Addition amount of auxiliary agent | 800ppm | 1000ppm | 300ppm |
| Temperature, C | 125 | 130 | 120 |
| Pressure, MPa | 1.2 | 1.25 | 1.2 |
TABLE 7 hydrogenation reaction conditions in suspended bed
| Item | Example 1 | Example 2 | Example 3 |
| Adding amount of molybdenum isooctanoate | 600ppm | 400ppm | 500ppm |
| Adding amount of carbon disulfide | 500ppm | 500ppm | 500ppm |
| Temperature, C | 420 | 370 | 380 |
| Pressure, |
16 | 16 | 16 |
| Space velocity, h -1 | 0.5 | 0.8 | 0.6 |
| Hydrogen to oil ratio, v/v | 1500 | 1000 | 1300 |
TABLE 8 suspension bed oil production results
| Item | Example 1 | Example 2 | Example 3 |
| Liquid phase yield% | 95.73 | 98.84 | 93.41 |
| Sulfur content, mg/kg | 126 | 331 | 17 |
| Nitrogen content, mg/kg | 3827 | 205 | 63 |
| Cl content, |
2 | 7 | 1 |
| Residual carbon content% | 0.01 | 0.04 | 0.01 |
| Ash content% | Trace amount of | Trace amount of | Trace amount of |
TABLE 9 fixed bed hydrogenation reaction conditions
Example 1 fixed bed hydrogenation of fuel oil fractions main product: the analytical indexes of the high-flash-point jet fuel and the light white oil are shown in the table 10 and the table 11.
TABLE 10 high flash point jet fuels
TABLE 11 light white oil
Example 1 base oil fraction fixed bed hydrogenation of the main products: the analytical indexes of the industrial white oil (II) No. 22 and the naphthenic mineral oil as the rubber plasticizer are shown in tables 12 and 13.
TABLE 12 technical white oil No. (II) 22
TABLE 13 rubber plasticizers naphthenic mineral oils
Example 2 fixed bed hydrogenation of fuel oil fraction main product: the analysis indexes of the light white oil W2-TA are shown in Table 14.
TABLE 14 light white oil
Example 2 base oil fraction fixed bed hydrogenation of main products: the analytical indexes of the technical white oil (II) No. 5 and the lubricating base oil are shown in tables 15 and 16.
TABLE 15 technical white oil No. (II) 5
TABLE 16 lubricating oil base oils (> 350 ℃ C. Fraction)
| Item | Analyzing data |
| Kinematic viscosity (40 ℃ C.), mm 2 /s | 32.41 |
| Kinematic viscosity (40 ℃ C.), mm 2 /s | 5.72 |
| Viscosity index | 118 |
| Pour point, DEG C | -24 |
| Flash point (open mouth),. Degree.C | 219 |
| Sulfur content, mg/L | ＜1 |
| Nitrogen content, mg/L | ＜1 |
Example 3 fixed bed hydrogenation of fuel oil fractions main product: the analysis indexes of the biological aviation kerosene are shown in the table 17.
TABLE 17 biological aviation kerosene
Example 3 base oil fraction fixed bed hydrogenation main product: the analytical indexes of the industrial white oil (II) No. 5 and the industrial white oil (II) No. 15 are shown in tables 18 and 19.
TABLE 18 technical white oil No. (II) 5
TABLE 19 technical white oil No. (II) 15
Claims (10)
1. A method for preparing jet fuel, white oil and lubricating oil base oil by hydrogenating waste oil is characterized by comprising the following steps:
step 1: waste oil mixing and pretreatment
According to the mass percentage, 5 to 85 percent of waste coal tar, 5 to 80 percent of rubber oil, 5 to 85 percent of waste mineral oil and 5 to 85 percent of waste biomass oil are mixed evenly in a component adjusting mixer (1) to obtain mixed waste oil; removing most of solid or insoluble impurities and water in the mixed waste oil by a centrifugal machine (2), heating the mixed waste oil to 100-150 ℃ in a heater (3), mixing the waste oil with a dehydration and desalination auxiliary agent, then feeding the mixture into a dehydration tank (4), maintaining the pressure in the dehydration tank (4) at 0.5-1.5 MPa, completing demulsification and dehydration of the mixed waste oil, feeding the dehydrated mixed waste oil into a flash evaporation and dehydration tower (5) for deep dehydration, and removing free water, emulsified water and salt in an oil phase;
step 2: hydrogenation in suspension bed
Adding an oil-soluble catalyst precursor and a vulcanizing agent into the deeply dehydrated mixed waste oil, boosting the pressure of the mixed waste oil by a high-pressure feed pump (6), mixing the mixture with hydrogen, feeding the mixture into a first heating furnace (7), heating the mixture by the first heating furnace (7), feeding the mixture into a suspension bed reactor (8), carrying out a suspension bed hydrogenation reaction in the suspension bed reactor (8), removing metals and residual carbon, and removing partial sulfur, nitrogen and oxygen to ensure that the metal removal rate in the mixed waste oil is greater than 95%, the residual carbon removal rate is greater than 94% and the sulfide removal rate is greater than 70%; the suspension bed hydrogenation product is separated into a gas phase and a liquid phase through a first high-pressure separator (9), the gas phase enters a first cold low-pressure separator (10) for further separation into hydrogen and naphtha, the liquid phase enters a first hot low-pressure separator (11) for further separation into naphtha and pre-hydrogenated distillate oil, the pre-hydrogenated distillate oil is sent into a first fractionating tower (12) for atmospheric and vacuum fractionation, and the naphtha, the fuel oil fraction at 180-320 ℃, the base oil fraction at 320-480 ℃ and the bottom reducing oil are fractionated; hydrogen separated by the first cold low-pressure separator (10) is recycled after being boosted by a recycle hydrogen compressor, naphtha separated by the first cold low-pressure separator (10) and the first hot low-pressure separator (11) and naphtha fractionated by the first fractionating tower (12) are output as products, fuel oil fraction and base oil fraction respectively enter a fuel oil fraction storage tank (14) and a base oil fraction storage tank (15), catalyst components mixed in the bottom-reducing oil and the bottom-reducing oil are boosted by a bottom-reducing oil circulating pump (13) and then are sent back to the suspension bed reactor (8), and the suspension bed hydrogenation reaction is continuously carried out; wherein the oil-soluble catalyst precursor is oil-soluble molybdenum isooctanoate;
and step 3: fixed bed hydrogenation
Mixing a fuel oil fraction in a fuel oil fraction storage tank (14) and a base oil fraction in a base oil fraction storage tank (15) with a vulcanizing agent and hydrogen respectively in an alternate feeding mode, then feeding the mixture into a second heating furnace (16) for heating, then feeding the mixture into a first refining reactor (17), carrying out deep hydrofining reaction in the first refining reactor (17), removing sulfur, nitrogen and aromatic hydrocarbon components, mixing a hydrofining product with the hydrogen, then feeding the mixture into an isomerization reactor (18), carrying out isomerization reaction in the isomerization reactor (18), carrying out heat exchange on the reacted oil by a heat exchanger (19), then feeding the reacted oil into a stripping tower (20), completing steam stripping of hydrogen sulfide and ammonia components dissolved in the oil in the stripping tower (20), mixing the stripped oil with new hydrogen, then feeding the mixed oil into a second refining reactor (21), carrying out deep hydrofining reaction in the second refining reactor (21), removing olefin and aromatic hydrocarbon components, after the reaction, feeding distillate oil from the second refining reactor (21) into a second high-pressure separator (22) for gas-liquid separation, feeding into a second low-pressure separator (23) for further cold-liquid phase separation, and further carrying out naphtha separation into a second naphtha separation, and further carrying out liquid-phase separation into a naphtha (24); naphtha separated by the second cold low-pressure separator (23) and the second hot low-pressure separator (24) is output as a product, hydrogen separated by the second cold low-pressure separator (23) is sent to the stripping tower (20) after being boosted by a recycle hydrogen compressor to be recycled as stripping gas, the content of sulfur and nitrogen in oil stripped by the stripping tower (20) is ensured to be less than 5ppm, and hydro-upgrading distillate oil separated by the second hot low-pressure separator (24) is sent to the second fractionating tower (25) to be fractionated into naphtha, jet fuel, white oil, lubricating oil base oil and rubber plasticizer cycloalkyl mineral oil products.
2. The process of claim 1 for the hydrogenation of waste oils to jet fuels, white oils and lubricant bases, characterized in that: in the step 1, when the total mass percent of the waste coal tar and the rubber oil accounts for 10-50% of the mixed waste oil, the products fractionated by the second fractionating tower (25) in the step 3 mainly comprise naphtha, biological aviation kerosene, industrial white oil and lubricating oil base oil; in the step 1, when the total mass percentage of the waste coal tar and the rubber oil accounts for 60-90% of the mixed waste oil, the products fractionated by the second fractionating tower (25) in the step 3 mainly comprise high-flash-point jet fuel, industrial white oil and naphthenic mineral oil as a rubber plasticizer.
3. The process for obtaining jet fuel, white oil and lubricant base oil by hydrogenating waste oil according to claim 1 or 2, wherein: in the step 1, the injection amount of the dehydration and desalination auxiliary agent is 100-1000 ppm.
4. A process for the preparation of jet fuel, white oil and lubricant base oil by hydrogenation of waste oil according to claim 1 or 2, characterized in that: in the step 2, the injection amount of the oil-soluble catalyst precursor is 100 ppm-1000 ppm, and the oil-soluble molybdenum isooctanoate is decomposed and sulfurized into the nano-scale molybdenum sulfide catalyst in situ in the hydrogen environment and is highly dispersed in the oil phase.
5. A process for the preparation of jet fuel, white oil and lubricant base oil by hydrogenation of waste oil according to claim 1 or 2, characterized in that: in the step 2, the hydrogenation reaction temperature of the suspension bed is 360-450 ℃, the reaction pressure is 12-18 MPa, and the volume space velocity is 0.5-1.3 h -1 The volume ratio of hydrogen to oil is 800-1500.
6. The process for obtaining jet fuel, white oil and lubricant base oil by hydrogenating waste oil according to claim 1 or 2, wherein: in the step 2 and the step 3, the injection amount of the vulcanizing agent is 100 to 500ppm.
7. The process of claim 1 for the hydrogenation of waste oils to jet fuels, white oils and lubricant bases, characterized in that: in step 3, when the fuel is onWhen the oil fraction is hydrogenated in a fixed bed, the deep hydrofining reaction temperature is 300-360 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 1000-1500, and the volume space velocity is 0.4-0.7 h -1 (ii) a The isomerization reaction temperature is 320-350 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 1000-2000, and the volume space velocity is 0.5-1.5 h -1 (ii) a The deep hydrogenation saturation reaction temperature is 150-200 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 500-1000 -1 。
8. The process of claim 1 for the hydrogenation of waste oils to jet fuels, white oils and lubricant bases, characterized in that: in step 3, when the base oil fraction is subjected to fixed bed hydrogenation, the deep hydrofining reaction temperature is 360-400 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 1200-2000, and the volume space velocity is 0.4-0.7 h -1 (ii) a The isomerization reaction temperature is 350-400 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 1000-2000 -1 (ii) a The deep hydrogenation saturation reaction temperature is 200-250 ℃, the reaction pressure is 8-20 MPa, the hydrogen-oil ratio is 500-1000 -1 。
9. The process of claim 1 for hydroprocessing a jet fuel, a white oil and a lubricant base oil from a waste oil, wherein: in step 3, the catalyst for the deep hydrofining reaction adopts phosphorus modified alumina with bimodal distribution of pore diameter as a carrier, and 2-3% of NiO and MoO are loaded on the carrier 3 5%～8%、WO 3 18 to 25 percent; the catalyst for the isomerization reaction takes silicon modified ZSM-5 as a carrier and loads 1.5 to 5 percent of NiO; the catalyst for the deep hydrogenation saturation reaction takes amorphous silicon-aluminum as a carrier and loads 8-15% of NiO; wherein, the loading amount of the active components is calculated by taking the mass of the catalyst as 100 percent.
10. A system for preparing jet fuel, white oil and lubricant base oil by hydrogenating waste oil by implementing the method of claim 1, which is characterized in that: the system mainly comprises a raw material pretreatment unit, a suspension bed hydrogenation unit and a fixed bed hydrogenation unit; wherein, the raw material pretreatment unit consists of a component adjusting mixer (1), a centrifuge (2), a heater (3), a dehydration tank (4) and a flash evaporation dehydration tower (5); the suspension bed hydrogenation unit is formed by connecting a high-pressure feed pump (6), a first heating furnace (7), a suspension bed reactor (8), a first high-pressure separator (9), a first cold low-pressure separator (10), a first hot low-pressure separator (11), a first fractionating tower (12), a bottom-reducing oil circulating pump (13), a fuel oil fraction storage tank (14) and a base oil fraction storage tank (15); the fixed bed hydrogenation unit is formed by connecting a second heating furnace (16), a first refining reactor (17), an isomerization reactor (18), a heat exchanger (19), a stripping tower (20), a second refining reactor (21), a second high-pressure separator (22), a second cold low-pressure separator (23), a second hot low-pressure separator (24) and a second fractionating tower (25);
the waste coal tar, the rubber oil, the waste biomass oil and the waste mineral oil pipeline are respectively communicated with a component adjusting mixer (1), and an outlet of the component adjusting mixer (1) is sequentially communicated with a centrifugal machine (2), a heater (3), a dehydration tank (4) and a flash evaporation dehydration tower (5); the bottom outlet of the flash dehydration tower (5) is connected with the inlet of a high-pressure feed pump (6), the outlet of the high-pressure feed pump (6) is connected with the inlet of a first heating furnace (7) after being converged with a first cold low-pressure separator (10) top outlet circulating hydrogen pipeline and a new hydrogen pipeline, the discharge port of the first heating furnace (7) is communicated with the bottom inlet of a suspended bed reactor (8) after being converged with a bottom oil circulating pump (13) outlet pipeline, the top outlet of the suspended bed reactor (8) is communicated with a first high-pressure separator (9), the top outlet of the first high-pressure separator (9) is communicated with a first cold low-pressure separator (10), the bottom outlet of the first cold low-pressure separator (10) and the top outlet of the first hot low-pressure separator (11) are both connected with a naphtha output pipeline, the bottom outlet of the first hot low-pressure separator (11) is communicated with a first fractionating tower (12), the bottom outlet of the first fractionating hot low-pressure separator (11) is communicated with a first fractionating tower (12), the first fractionating tower (12) is connected with the inlet of the bottom outlet of the bottom oil circulating pump (10) and the first hot low-pressure separator (11), the top outlet of the fractionating tower (12) is communicated with a second fractionating tower bottom outlet of a base oil circulating pump (14) and a second fractionating tower, the outlet of the base oil circulating fuel oil storage tank (14) is respectively communicated with a second fractionating tower (15), the bottom outlet of the base oil storage tank (15) and the base oil storage tank (15), the base oil storage tank (15) after being communicated with a second fractionating tower, the hydrogen storage tank (15) and the base oil storage tank (15), the base oil storage tank (storage tank, the base oil storage tank (15) and the base oil storage tank, the outlet of the base oil storage tank (15) of the base oil storage tank The ports are communicated; the discharge hole of the second heating furnace (16) is communicated with the top inlet of the first refining reactor (17), the bottom outlet of the first refining reactor (17) is communicated with the fresh hydrogen pipeline and the top outlet of the stripping tower (20) through the circulating hydrogen pipeline after being converged and then communicated with the top inlet of the isomerization reactor (18), the bottom outlet of the isomerization reactor (18) is communicated with the middle inlet of the stripping tower (20) through a heat exchanger (19), the bottom outlet of the stripping tower (20) is communicated with the top inlet of the second refining reactor (21) after being converged and then communicated with the top outlet of the second refining reactor (21), the bottom outlet of the second refining reactor (21) is communicated with the second high-pressure separator (22), the top outlet of the second high-pressure separator (22) is communicated with the second cold low-pressure separator (23), the bottom outlet of the second high-pressure separator (22) is communicated with the second hot low-pressure separator (24), the bottom outlet of the second hot low-pressure separator (24) is communicated with the lower part of the second dividing tower (25), and the bottom outlet of the second cold low-pressure separator (23) and the top outlet of the second hot low-pressure separator (24) are both connected with the naphtha output pipeline.
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| US12084621B1 (en) * | 2023-04-19 | 2024-09-10 | Sk Innovation Co., Ltd. | Method and system for producing refined hydrocarbons from waste plastic pyrolysis oil |
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| US20240352351A1 (en) * | 2023-04-19 | 2024-10-24 | Sk Innovation Co., Ltd. | Method and system for producing refined hydrocarbons from waste plastic pyrolysis oil |
| US12258525B2 (en) * | 2023-04-19 | 2025-03-25 | Sk Innovation Co., Ltd. | Method and system for producing refined hydrocarbons from waste plastic pyrolysis oil |
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| US20240352342A1 (en) * | 2023-04-19 | 2024-10-24 | Sk Innovation Co., Ltd. | Method and system for producing refined hydrocarbons from waste plastic pyrolysis oil |
| CN118931591A (en) * | 2024-08-15 | 2024-11-12 | 上海汉兴化工科技有限公司 | A system and method for treating waste mineral oil in the presence of hydrogen |
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