CN108977224A - Transformer oil base oil and preparation method thereof - Google Patents
Transformer oil base oil and preparation method thereof Download PDFInfo
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- CN108977224A CN108977224A CN201810865649.8A CN201810865649A CN108977224A CN 108977224 A CN108977224 A CN 108977224A CN 201810865649 A CN201810865649 A CN 201810865649A CN 108977224 A CN108977224 A CN 108977224A
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- 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
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- 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
- C10G2400/12—Electrical isolation oil
Abstract
The present invention provides a kind of transformer oil base oils and preparation method thereof.The preparation method includes: 1) to be fractionated coal direct liquefaction oil, obtains diesel oil distillate, and the boiling range of diesel oil distillate is 290~330 DEG C；2) diesel oil distillate is subjected to hydrofining reaction, obtains hydrogenation products；3) hydrogenation products are subjected to hydro-upgrading reaction, obtain the first transformer oil base oil；4) first transformer oil base oil is subjected to hydrofining reaction, obtains the second transformer oil base oil；Wherein coal direct liquefaction oil includes oil A and oil B, wherein the volume ratio of oil A and the oil B are 1:1~1:10, wherein oil A by weight percentage and oil B includes a certain amount of alkane, cycloalkane, mononuclear aromatics, double ring arene and thrcylic aromatic hydrocarbon, and the sum of each component content is equal to 100%.The preparation method process flow is short, and low energy consumption and target product yield is high, performance is all good.
Description
Technical field
The present invention relates to petrochemical industries, in particular to a kind of transformer oil base oil and preparation method thereof.
Background technique
Transformer oil refers in the oil-filled electric equipments such as transformer, reactor, mutual inductor, casing, oil circuit breaker, rises exhausted
A kind of liquid insulating material that edge, cooling and arc extinguishing act on.The main function of transformer oil include insulation protection, shine heat it is cooling and
Arc extinguishing, therefore the requirement of the electric property and physicochemical property to transformer oil is especially high.It is cold in the important performance of transformer oil
But heat dissipation performance, solubility property, anti-oxidant, ageing properties, electric property, cryogenic property and anti-gassing property energy, the hydrocarbon with oil product
Class composition has close connection.
Transformer oil base oil is the raw material for producing transformer oil.The performance of transformer oil depends greatly on change
The performance of depressor oil base oil.In general, paraffinic base transformer oil base oil pour point is high, the oxidizable a large amount of acid chemical combination of production
Object, and arene content is few, transformer oil service life, it is anti-oxidant, anti-in terms of come with some shortcomings.And naphthenic base transformation
Viscosity is low at high temperature for device oil base oil, and the solvability under extremely low temperature is excellent, and has very high oxidation stability, pole
Good electrical characteristic and good heat transfer medium characteristic had not only been able to satisfy the requirement such as insulation, cooling of transformer oil, but also can grow
Phase steady operation, therefore become the optimum feed stock of acknowledged production transformer oil base oil.Currently, global transformer manufacturing
The large multinational companies such as quotient, especially ABB, Alstom transformer produced, uses bar none with naphthenic base oils
The transformer oil of production.
The raw material of traditional naphthenic base transformer foundation oil is naphthene base crude.But the reserves of one side naphthene base crude are only
The 2%~3% of crude oil gross reserves is accounted for, and the main place of production is on the U.S., Venezuela and other places.The naphthene base crude in another aspect China
Only Karamay, Xinjiang keeps the stabilization output of naphthenic base transformer oil base oil, other producing regions such as Liaohe Huanxiling in main product ground
And Bohai Sea Gulf cannot function as the stable resources of production transformer oil with yield reduction and quality variation.With China's electricity
The development of Lixing sparetime university and the Domestic Transformers oil market demand constantly increase, and imbalance between supply and demand is more prominent, therefore developing is other suitable
Transformer oil raw materials for production, realize transformer oil significantly domesticize, be of great immediate significance.
Important leverage of the direct coal liquefaction technology as China's energy, product direct liquefaction oil have sulphur, nitrogen content low,
The high characteristic of arene content, how according to its product characteristic, the comprehensive utilization for efficiently carrying out coal direct liquefaction oil is to promote its warp
The important link of Ji property.Coal direct liquefaction oil can be transformed into cycloalkane after hydrotreating and hydro-upgrading.
The preparation method of transformer oil base oil in the prior art mainly has the defect of following several respects:
Defect one: long technical process, at high cost, target product yield is low, poor continuity, treating capacity is small and naphthenic base evaporates
Divide oily resource limited.
Defect two: a large amount of environmental pollution (such as acid sludge, nitrogen slag, clay dregs) is generated.
Based on the above reasons, it needs further to study the preparation method of transformer oil base oil, to solve its work
Skill process is long, at high cost, target product yield is low, poor continuity, treating capacity is small and naphthenic base distillate resource is limited and produces
The problem of raw a large amount of environmental pollution (such as acid sludge, nitrogen slag, clay dregs).
Summary of the invention
The main purpose of the present invention is to provide a kind of transformer oil base oils and preparation method thereof, to solve the prior art
In preparation method long technical process, at high cost, target product yield is low, poor continuity, treating capacity are small and naphthenic base fraction
Oily resource is limited and leads to the problem of a large amount of environmental pollution (such as acid sludge, nitrogen slag, clay dregs).
To achieve the goals above, according to an aspect of the invention, there is provided a kind of preparation of transformer oil base oil
Method, the preparation method include: 1) to be fractionated coal direct liquefaction oil, obtain diesel oil distillate, and the boiling range of the diesel oil distillate is
290~330 DEG C；2) diesel oil distillate is subjected to hydrofining reaction, obtains hydrogenation products；3) hydrogenation products are carried out adding hydrogen
Modification reaction, obtains the first transformer oil base oil；4) first transformer oil base oil is subjected to hydrofining reaction,
Obtain the second transformer oil base oil；Wherein the coal direct liquefaction oil includes oil A and oil B, wherein the volume of oil A and oil B
Than for 1:1~1:10, wherein oil A by weight percentage includes 5%~15% alkane, 25%~35% cycloalkanes
Hydrocarbon, 50%~60% mononuclear aromatics, 10%~20% double ring arene, 0%~10% thrcylic aromatic hydrocarbon, each component content it
Be equal to 100%, wherein oil B by weight percentage comprising 0%~15% alkane, 5%~20% cycloalkane,
40%~55% mononuclear aromatics, 35%~50% double ring arene, 5%~20% thrcylic aromatic hydrocarbon, the sum of each component content
Equal to 100%.
Further, the reaction pressure of the hydrofining reaction in step 2) is 3.0~21.0MPa.
Further, the reaction pressure of the hydrofining reaction in step 2) is 10.0~15.0MPa.
Further, the reaction temperature of the hydrofining reaction in step 2) is 250~400 DEG C.
Further, the reaction temperature of the hydrofining reaction in step 2) is 300~350 DEG C.
Further, the volume ratio of the hydrogen of the hydrofining reaction in step 2) and the diesel oil distillate be 400:1~
2000:1。
Further, the volume ratio of the hydrogen of the hydrofining reaction in step 2) and the diesel oil distillate be 800:1~
1200:1。
Further, the volume space velocity of the hydrofining reaction in step 2) is 0.1~2.5h-1。
Further, the volume space velocity of the hydrofining reaction in step 2) is 0.5~1.0h-1。
Further, the reaction pressure of the hydro-upgrading reaction in step 3) is 3.0~21.0MPa.
Further, the reaction pressure of the hydro-upgrading reaction in step 3) is 10.0~15.0MPa.
Further, the reaction temperature of the hydro-upgrading reaction in step 3) is 250~400 DEG C.
Further, the reaction temperature of the hydro-upgrading reaction in step 3) is 300~340 DEG C.
Further, in step 3) the hydro-upgrading reaction hydrogen and the hydrogenation products volume ratio be 400:1~
2000:1。
Further, in step 3) the hydro-upgrading reaction hydrogen and the hydrogenation products volume ratio be 800:1~
1200:1。
Further, the volume space velocity of the hydro-upgrading reaction in step 3) is 0.1~2.5h-1。
Further, the volume space velocity of the hydro-upgrading reaction in step 3) is 0.8~1.5h-1。
Further, the reaction pressure of the hydrofining reaction in step 4) is 3.0~15.0MPa.
Further, the reaction pressure of the hydrofining reaction in step 4) is 6~15.0MPa.
Further, the reaction temperature of the hydrofining reaction in step 4) is 140~300 DEG C.
Further, the reaction temperature of the hydrofining reaction in step 4) is 160~220 DEG C.
Further, the body of the hydrogen and first transformer oil base oil of the hydrofining reaction in step 4)
Product is than being 200:1~2000:1.
Further, the body of the hydrogen and first transformer oil base oil of the hydrofining reaction in step 4)
Product is than being 400:1~1000:1.
Further, the volume space velocity of the hydrofining reaction in step 4) is 0.1~2.5h-1。
Further, the volume space velocity of the hydrofining reaction in step 4) is 0.6~1.5h-1。
Further, the volume ratio of oil A and oil B is 1:2~1:8.
Further, the volume ratio of oil A and oil B is 1:3~1:7.
Further, the volume ratio of oil A and oil B is 1:4~1:6.
Further, the volume ratio of oil A and oil B is 1:6.
Further, oil A by weight percentage include 5%~10% alkane, 25%~30% cycloalkane,
50%~55% mononuclear aromatics, 10%~15% double ring arene, 0%~5% thrcylic aromatic hydrocarbon.
Further, oil A by weight percentage include 5%~7% alkane, 28%~30% cycloalkane,
50%~55% mononuclear aromatics, 10%~15% double ring arene, 0%~2% thrcylic aromatic hydrocarbon.
Further, oil B by weight percentage include 0%~10% alkane, 5%~15% cycloalkane,
40%~50% mononuclear aromatics, 35%~45% double ring arene, 5%~15% thrcylic aromatic hydrocarbon.
Further, oil B by weight percentage include 0%~5% alkane, 5%~10% cycloalkane,
40%~45% mononuclear aromatics, 35%~40% double ring arene, 5%~10% thrcylic aromatic hydrocarbon.
Further, in step 2), hydrogenation protecting catalyst and Hydrobon catalyst are used.
Further, in step 2), the admission space ratio of the hydrogenation protecting catalyst and the Hydrobon catalyst is
1:2~1:6.
Further, in step 2), the admission space ratio of the hydrogenation protecting catalyst and the Hydrobon catalyst is
1:4。
Further, in step 2), which is RGC-1 series hydrogenation protecting catalyst and/or FZC
Serial hydrogenation protecting catalyst.
Further, in step 2), which is to be with porous refractory inorganic oxide such as aluminium oxide
The oxide of carrier, group VIB and/or group VIII metal such as W, Mo, Co, Ni as active component, optionally containing P, Si,
F, the catalyst of B.
Further, in step 2), which is RNC-2 series Hydrobon catalyst and/or FF-
26 serial Hydrobon catalysts.
Further, in step 2), the active component of the Hydrobon catalyst is group VIB and/or group VIII
The oxide of metal such as W, Mo, Co, Ni.
Further, in step 2), the Hydrobon catalyst includes 15~30% Section VI B by weight percentage
Family metal oxide.
Further, in step 2), the Hydrobon catalyst includes 2~6% Section VIII by weight percentage
Family metal oxide.
Further, in step 2), the specific surface of the Hydrobon catalyst is >=100m2/g。
Further, in step 2), the pore volume of the Hydrobon catalyst is >=0.24ml/g.
Further, in step 3), catalyst for hydro-upgrading is used.
Further, in step 3), which is RCC-1 series catalyst for hydro-upgrading and/or FC-
28 serial catalyst for hydro-upgrading.
Further, in step 3), the active component of the catalyst for hydro-upgrading is group VIB and/or group VIII
The oxide of metal such as W, Mo, Co, Ni.
Further, in step 3), the Hydrobon catalyst includes 10~30% Section VI B by weight percentage
Family metal oxide.
Further, in step 3), the Hydrobon catalyst includes 4~10% Section VIII by weight percentage
Family metal oxide.
Further, in step 3), the specific surface area of the catalyst for hydro-upgrading is >=200m2/g。
Further, in step 3), 0.2~0.7mL/g of Kong Rongwei of the catalyst for hydro-upgrading.
Further, in step 3), the Kong Rong of 3~10nm of bore dia of the catalyst for hydro-upgrading accounts for total pore volume
70%~95%.
Further, in step 3), the Kong Rong of 3~10nm of bore dia of the catalyst for hydro-upgrading accounts for total pore volume
85%~95%.
Further, in step 3), the infrared acidity of the catalyst for hydro-upgrading is 0.2~0.6mmol/g.
Further, in step 4), hydrofining catalyst is used.
Further, in step 4), which is RLF-20 series hydrofining catalysis
Agent and/or FMTA-2 series hydrofining catalyst.
Further, in step 4), the active component of the hydrofining catalyst be group VIII metal such as Pd,
The oxide of Pt.
Further, in step 4), the hydrofining catalyst includes 0.1%~2% by weight percentage
Group VIII metal oxide.
Further, in step 4), by weight percentage the hydrofining catalyst include 0.1%~
0.8% Pd oxide and 0.1%~0.5% Pt oxide.
Further, in step 4), the specific surface area of the hydrofining catalyst is >=200m2/g。
Further, in step 4), Kong Rongwei >=0.5mL/g of the hydrofining catalyst.
Further, in step 4), the bore dia of the hydrofining catalyst is >=8nm.
Further, in step 4), the active metal H of the hydrofining catalyst2Adsorbance is >=80mL/g.
According to another aspect of the present invention, a kind of transformer oil base oil prepared by above-mentioned preparation method is provided.
Apply the technical scheme of the present invention, the preparation method of transformer oil base oil include: 1) by coal direct liquefaction oil into
Row fractionation, obtains diesel oil distillate, and the boiling range of the diesel oil distillate is 290~330 DEG C；2) diesel oil distillate progress hydrofinishing is anti-
It answers, obtains hydrogenation products；3) hydrogenation products are subjected to hydro-upgrading reaction, obtain the first transformer oil base oil；4) should
First transformer oil base oil carries out hydrofining reaction, obtains the second transformer oil base oil；The wherein direct liquid of the coal
Carburetion includes oil A and oil B, and wherein the volume ratio of oil A and oil B is 1:1~1:10, wherein oil A by weight percentage
Include 5%~15% alkane, 25%~35% cycloalkane, 50%~60% mononuclear aromatics, 10%~20% pair
Cycloaromatics, 0%~10% thrcylic aromatic hydrocarbon, the sum of each component content is equal to 100%, wherein oil B packet by weight percentage
Containing 0%~15% alkane, 5%~20% cycloalkane, 40%~55% mononuclear aromatics, 35%~50% bicyclic virtue
Hydrocarbon, 5%~20% thrcylic aromatic hydrocarbon, the sum of each component content are equal to 100%.The preparation method process flow is short, and low energy consumption simultaneously
And target product yield is high, the physical property of the transformer oil base oil of acquisition meets transformer oil standard, electric property, oxidation peace
Qualitative and anti-gassing property can be all good.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.
Fig. 1 shows of the invention with coal direct liquefaction oil production naphthenic base transformer oil base oil process flow signal
Figure.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.The present invention will be described in detail below with reference to the accompanying drawings and embodiments.
The application is described in further detail below in conjunction with specific embodiment, these embodiments should not be understood as limitation originally
Apply for range claimed.
As described in background technology part, the preparation method of existing transformer oil base oil can not solve its technique
Process is long, at high cost, target product yield is low, poor continuity, treating capacity is small and naphthenic base distillate resource is limited and generates
The problem of a large amount of environmental pollution (such as acid sludge, nitrogen slag, clay dregs).To solve the above-mentioned problems, the present invention provides one kind
The preparation method of transformer oil base oil, the preparation method include: 1) to be fractionated coal direct liquefaction oil, obtain diesel oil and evaporate
Point, the boiling range of the diesel oil distillate is 290~330 DEG C；2) diesel oil distillate is subjected to hydrofining reaction, obtains hydrogenation products；
3) hydrogenation products are subjected to hydro-upgrading reaction, obtain the first transformer oil base oil；4) by first transformer oil basis
Oil carries out hydrofining reaction, obtains the second transformer oil base oil；Wherein the coal direct liquefaction oil includes oil A and oil B,
Wherein the volume ratio of oil A and oil B is 1:1~1:10, wherein oil A by weight percentage includes 5%~15% chain
Alkane, 25%~35% cycloalkane, 50%~60% mononuclear aromatics, 10%~20% double ring arene, 0%~10%
Thrcylic aromatic hydrocarbon, the sum of each component content are equal to 100%, wherein oil B by weight percentage includes 0%~15% alkane
Hydrocarbon, 5%~20% cycloalkane, 40%~55% mononuclear aromatics, 35%~50% double ring arene, the three of 5%~20%
Cycloaromatics, the sum of each component content are equal to 100%.
In the method for the present invention, the step 1) coal direct liquefaction oil fractionation after gained < 160 DEG C may be used as gasoline reconciliation group
Point, 160~290 DEG C of blend components that may be used as diesel oil, > 330 DEG C of fractions may be used as processing refrigerator oil, rubber filling oil
Deng the feedstock oil of other lube base oils.
The preparation method process flow is short, and low energy consumption and target product yield is high, the transformer oil base oil of acquisition
Physical property meets transformer oil standard, and electric property, oxidation stability and anti-gassing property can be all good.
Specifically, compared with prior art, preparation method of the invention has the advantages that
(1) present invention produces transformer oil base oil by raw material of coal direct liquefaction oil for the first time, for mentioning for direct liquefaction oil
Matter effectively extends the industrial chain that direct liquefaction oil product utilizes using a new way is opened.The direct liquefaction process of coal
It is hydrogenation process, generated liquefaction oil have passed through hydroprocessing processes again, so its oil product has relative clean, metal
Impurity and the low feature of water content, compare the processing for being suitable as downstream base oil.Therefore, transformation is produced with coal direct liquefaction oil
Device oil base oil has process flow short, and low energy consumption, good product quality, and the advantage that target product yield is high.
(2) present invention passes through hydrofinishing first by (290-330 DEG C) the progress hydrotreating of coal direct liquefaction oil distillate
It can be saturated with desulfurization, denitrogenation and aromatic moiety.Simultaneously by hydro-upgrading, saturation is carried out to two rings and a small amount of thrcylic aromatic hydrocarbon and is opened
Ring, while the complete of open loop rear side chain is kept, become the monocycle or two cycloaromatics of belt length side chain, by hydro-upgrading and hydrogen is added to mend
After filling purification, the cycloalkane largely with more side chains is generated, electric property, oxidation stability and anti-gassing property can be obtained can be all good
Transformer oil base oil.There is a small amount of linear paraffin isomery centainly influenced at branched paraffin on condensation point simultaneously, guarantees product
Cryogenic property.
(3) the method for the present invention provides a kind of processing method for improving its economy, Er Qiewei for coal direct liquefaction oil
A kind of new raw material of the production development of transformer oil base oil.The energy resource structure in China is rich coal oil starvation, DCL/Direct coal liquefaction conduct
Chinese energy safety ensures a strategic important supplement means, is forming industrialized scale, and coal direct liquefaction oil is rich in
Aromatic hydrocarbons and cycloalkane, therefore go out to utilize the method for the present invention that can substitute rare naphthene base crude resource, produce China's electric power
The high-quality transformer oil base oil that industry is badly in need of can simultaneously be effectively promotes the reasonable utilization of DCL/Direct coal liquefaction oil product.
(4) other fractions after the method for the present invention hydrotreating can be used as the blend component or other of gasoline and diesel oil
The raw material of specialty oil.
In a preferred embodiment, the reaction pressure of the hydrofining reaction in step 2) be 3.0~
21.0MPa, preferably 10.0~15.0MPa；Reaction temperature is 250~400 DEG C, preferably 300~350 DEG C；Hydrogen and the diesel oil
The volume ratio of fraction is 400:1~2000:1, preferably 800:1~1200:1；Volume space velocity is 0.1~2.5h-1, preferably
0.5~1.0h-1.Relative to the reaction condition of other hydrofining reactions, above-mentioned hydrofining reaction used in this application
Reaction condition can more efficiently by the objectionable impurities such as sulphur, oxygen, nitrogen in coal direct liquefaction oil be changed into corresponding hydrogen sulfide,
Water, ammonia and remove, and make that alkene and diene hydrogenation are saturated, aromatic moiety adds hydrogen to be saturated, to preferably improve the direct liquid of coal
The quality of carburetion.
In a preferred embodiment, in step 3) the hydro-upgrading reaction reaction pressure be 3.0~
21.0MPa, preferably 10.0~15.0MPa；Reaction temperature is 250~400 DEG C, preferably 300~340 DEG C；Hydrogen adds with this
The volume ratio of hydrogen product is 400:1~2000:1, preferably 800:1~1200:1；Volume space velocity is 0.1~2.5h-1, preferably
0.8~1.5h-1.Relative to the reaction condition of other hydro-upgradings reaction, above-mentioned hydro-upgrading reaction used in this application
Reaction condition preferably improves the Cetane number of coal direct liquefaction oil, reduces coal direct liquefaction oil condensation point, density.
In a preferred embodiment, in step 4) the hydrofining reaction reaction pressure be 3.0~
15.0MPa, preferably 6~15.0MPa；Reaction temperature is 140~300 DEG C, preferably 160~220 DEG C；Hydrogen and first change
The volume ratio of depressor oil base oil is 200:1~2000:1, preferably 400:1~1000:1；Volume space velocity is 0.1~2.5h-1,
Preferably 0.6~1.5h-1.Relative to the reaction condition of other hydrofinings reaction, above-mentioned plus hydrogen used in this application
The reaction condition of post-refining reaction is preferably decreased obviously condensed-nuclei aromatics content, and is obviously improved electric property.
In order to further balance the effect between each component, in a preferred embodiment, oil A and oil B's
Volume ratio is 1:2~1:8, preferably 1:3~1:7, preferably 1:4~1:6, preferably 1:6；Preferably by weight percentage
Oil A include 5%~10% alkane, 25%~30% cycloalkane, 50%~55% mononuclear aromatics, 10%~15%
Double ring arene, 0%~5% thrcylic aromatic hydrocarbon, preferably by weight percentage oil A include 5%~7% alkane,
28%~30% cycloalkane, 50%~55% mononuclear aromatics, 10%~15% double ring arene, 0%~2% three cyclophanes
Hydrocarbon, preferably by weight percentage oil B include 0%~10% alkane, 5%~15% cycloalkane, 40%~
50% mononuclear aromatics, 35%~45% double ring arene, 5%~15% thrcylic aromatic hydrocarbon, preferably by weight percentage
Oil B includes 0%~5% alkane, 5%~10% cycloalkane, 40%~45% mononuclear aromatics, and 35%~40%
Double ring arene, 5%~10% thrcylic aromatic hydrocarbon.
In a preferred embodiment, in step 2), hydrogenation protecting catalyst and Hydrobon catalyst are used；
Preferably the admission space ratio of the hydrogenation protecting catalyst and the Hydrobon catalyst is 1:2~1:6, preferably 1:4.Relatively
In the admission space ratio of other hydrogenation protecting catalysts and Hydrobon catalyst, above-mentioned hydrogenation protecting used in this application
The admission space ratio of catalyst and Hydrobon catalyst can effectively clean, and preferably improve the matter of coal direct liquefaction oil
Amount.
In a preferred embodiment, in step 2), which is Petroleum Chemical Engineering Institute
(RIPP) the RGC-1 series hydrogenation protecting catalyst of development and production and/or Fushun Petrochemical Research Institute (FRIPP) development and production
FZC series hydrogenation protecting catalyst；Preferably the hydrogenation protecting catalyst is with porous refractory inorganic oxide such as aluminium oxide
For carrier, the oxide of group VIB and/or group VIII metal such as W, Mo, Co, Ni as active component, optionally containing P,
The catalyst of Si, F, B.Relative to other hydrogenation protecting catalysts, above-mentioned hydrogenation protecting catalyst used in this application can
Effective filter is miscellaneous and salt, effectively adsorbs in raw material to the harmful substance of major catalyst, such as heavy metal avoids host agent from permanently losing
It is living.
In a preferred embodiment, in step 2), which is Petroleum Chemical Engineering Institute
(RIPP) the RNC-2 series Hydrobon catalyst of development and production and/or Fushun Petrochemical Research Institute (FRIPP) development and production
FF-26 series Hydrobon catalyst；Preferably the active component of the Hydrobon catalyst is group VIB and/or the
The oxide of group VIII metal such as W, Mo, Co, Ni；Preferably by weight percentage the Hydrobon catalyst include 15~
30% vib metals oxide；Preferably by weight percentage the Hydrobon catalyst include 2~6% the
Group VIII metal oxide；Preferably the specific surface of the Hydrobon catalyst is >=100m2/g；Preferably the hydrofinishing is urged
The pore volume of agent is >=0.24ml/g.Relative to other Hydrobon catalysts, above-mentioned hydrofinishing used in this application
Catalyst can more efficiently by the objectionable impurities such as sulphur, oxygen, nitrogen in coal direct liquefaction oil be changed into corresponding hydrogen sulfide,
Water, ammonia and remove, and make that alkene and diene hydrogenation are saturated, aromatic moiety adds hydrogen to be saturated, to preferably improve the direct liquid of coal
The quality of carburetion.
In a preferred embodiment, in step 3), catalyst for hydro-upgrading is used；The preferably hydro-upgrading
Catalyst is that the RCC-1 series catalyst for hydro-upgrading of Petroleum Chemical Engineering Institute (RIPP) development and production or Fushun petrochemical industry are ground
Study carefully the FC-28 series catalyst for hydro-upgrading of institute (FRIPP) development and production；The preferably active component of the catalyst for hydro-upgrading
For group VIB and/or the oxide of group VIII metal such as W, Mo, Co, Ni；Preferably hydrofinishing by weight percentage
Catalyst includes 10~30% vib metals oxide；The preferably Hydrobon catalyst packet by weight percentage
Containing 4~10% group VIII metal oxide；Preferably the specific surface area of the catalyst for hydro-upgrading is >=200m2/g；It is excellent
0.2~0.7mL/g of Kong Rongwei of the selection of land catalyst for hydro-upgrading；Preferably the bore dia 3 of the catalyst for hydro-upgrading~
The Kong Rong of 10nm accounts for the 70%~95% of total pore volume；The preferably Kong Rongzhan of 3~10nm of bore dia of the catalyst for hydro-upgrading
The 85%~95% of total pore volume；Preferably the infrared acidity of the catalyst for hydro-upgrading is 0.2~0.6mmol/g.Relative to it
Its catalyst for hydro-upgrading, above-mentioned catalyst for hydro-upgrading used in this application preferably improve the 16 of coal direct liquefaction oil
Alkane value reduces coal direct liquefaction oil condensation point, density.
In a preferred embodiment, in step 4), hydrofining catalyst is used；Hydrogen should preferably be added
Post-refining catalyst be Petroleum Chemical Engineering Institute (RIPP) development and production RLF-20 series hydrofining catalyst and/
Or the FMTA-2 series hydrofining catalyst of Fushun Petrochemical Research Institute (FRIPP) development and production；Should preferably it add
The active component of hydrogen post-refining catalyst is the oxide of group VIII metal such as Pd, Pt；Preferably by weight percentage
The hydrofining catalyst includes 0.1%~2% group VIII metal oxide；Preferably by weight percentage should
Hydrofining catalyst includes 0.1%~0.8% Pd oxide and 0.1%~0.5% Pt oxide；Preferably should
The specific surface area of hydrofining catalyst is >=200m2/g；The preferably Kong Rongwei of the hydrofining catalyst >=
0.5mL/g；Preferably the bore dia of the hydrofining catalyst is >=8nm；The preferably hydrofining catalyst
Active metal H2Adsorbance is >=80mL/g.Relative to other hydrofining catalyst, used in this application is above-mentioned
Hydrofining catalyst is preferably decreased obviously condensed-nuclei aromatics content, and is obviously improved electric property.
The process flow diagram of the above-mentioned preparation method of the present invention can be as shown in Figure 1, coal direct liquefaction oil 1 enters fractionation
Tower 2 respectively obtains 3,160~290 DEG C of less than 160 DEG C fractions, 4,290~330 DEG C of fraction fraction 5 and is greater than 330 DEG C of fractions 6.Its
In, less than 160 DEG C fractions 3 can do gasoline blend component, and 160~290 DEG C of fractions 4 can do diesel oil blending component, be greater than
330 DEG C of fractions 6 can further cut former as refrigerator oil base oil raw material, rubber filling oil raw material or environment-friendly type aromatic naphtha
Material.290~330 DEG C of fractions 5 contact in the presence of hydrogen 8 with Hydrobon catalyst into hydrofining reaction area 7, carry out
Desulfurization, denitrogenation, aromatic hydrocarbons depth saturated reaction reduce arene content, guarantee the oxidation stability index of product.Hydrofining reaction
Product 9 enters hydro-upgrading reaction zone 10, carries out saturation open loop to two rings and a small amount of thrcylic aromatic hydrocarbon, while keeping chain on rear side of open loop
It is complete, become the monocycle with more side chains or two cycloaromatics.Then hydro-upgrading product 11 isolates gas 13 through separator 12
Afterwards, liquid product 14 enters the further saturation of progress aromatic hydrocarbons after hydrofining reactor 16 and the mixing of hydrogen 15, reduces
The above arene content of tricyclic, after post-refining product 17 isolates a small amount of byproduct 19 and tail gas 24 into fractionating column 18, liquid phase
After product 20 isolates a small amount of byproduct 22 into vacuum tower 21, transformer oil base oil product 23 is obtained.
In addition, according to another aspect of the present invention, providing a kind of transformer oil basis prepared by above-mentioned preparation method
Oil.
The physical property of the transformer oil base oil prepared by above-mentioned preparation method meets transformer oil standard, electric property,
Oxidation stability and anti-gassing property can be all good.
Beneficial effects of the present invention are further illustrated by the following examples:
Various catalyst involved in embodiment can select commercial catalyst by property, can also be by ability domain knowledge system
It is standby.The RGC- of the commercial catalysts that the hydrogenation protecting agent of hydroprocessing processes can choose such as Petroleum Chemical Engineering Institute's development and production
1 serial hydrogenation protecting agent；The commercial catalysts that Hydrobon catalyst can choose such as Petroleum Chemical Engineering Institute's development and production
RNC-2 series Hydrobon catalyst；The commercial catalysts that catalyst for hydro-upgrading can choose such as Petroleum Chemical Engineering Institute grinds
Make the RCC-1 range of commercial products catalyst for hydro-upgrading of production；The development and production of hydrofining catalyst Petroleum Chemical Engineering Institute
RLF-20 range of commercial products hydrofining catalyst.
Embodiment 1
Using Shenhua coal direct liquefaction oil as raw material, (coal direct liquefaction oil is by medium temperature oil and high temperature oil according to 1:6 mixing preparation
Into), the specific nature of medium temperature oil and high temperature oil is shown in Table 1.It loads hydrogenation protecting catalyst RGC-1 and adds in hydrofining reaction area
The admission space ratio of hydrogen catalyst for refining RNC-2, hydrogenation protecting catalyst RGC-1 and Hydrobon catalyst RNC-2 are 1:4.
Hydro-upgrading reaction zone loads catalyst for hydro-upgrading RCC-1.Hydrofining reaction zone loads hydrofining catalysis
Agent RLF-20.The process conditions and product property of hydrogenation process are shown in Table 2 and table 3.
Embodiment 2
Using Shenhua coal direct liquefaction oil as raw material, (coal direct liquefaction oil is by medium temperature oil and high temperature oil according to 1:1 mixing preparation
Into), remaining is same as Example 1, and the process conditions and product property of hydrogenation process are shown in Table 2 and table 3.
Embodiment 3
Using Shenhua coal direct liquefaction oil as raw material, (coal direct liquefaction oil is by medium temperature oil and high temperature oil according to 1:10 mixing preparation
Into), remaining is same as Example 1, and the process conditions and product property of hydrogenation process are shown in Table 2 and table 3.
Embodiment 4
Load hydrogenation protecting catalyst FZC and Hydrobon catalyst FF-26, hydrogenation protecting catalysis in hydrofining reaction area
The admission space of agent RGC-1 and Hydrobon catalyst RNC-2 ratio are 1:6, remaining is same as Example 1, the work of hydrogenation process
Skill condition and product property are shown in Table 2 and table 3.
Embodiment 5
It is FC-28 that hydro-upgrading reaction zone, which loads catalyst for hydro-upgrading, remaining is same as Example 1, hydrogenation process
Process conditions and product property are shown in Table 2 and table 3.
Embodiment 6
It is FMTA-2 that hydrofining reaction zone, which loads hydrofining catalyst, remaining is same as Example 1, adds
The process conditions and product property of hydrogen process are shown in Table 2 and table 3.
Comparative example 1
Using raw material same as Example 1, difference is hydrotreated product without hydro-upgrading, hydrogenation process
Process conditions and product property be shown in Table 2 and table 3.
Comparative example 2
Using raw material same as Example 1, difference is hydro-upgrading product without hydrofining, adds hydrogen
The process conditions and product property of process are shown in Table 2 and table 3.
1 coal direct liquefaction oil physical property of table
The process conditions of table 2 embodiment and comparative example
| Experiment numbers | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 |
| Hydrofining technology condition | |||||
| Reaction temperature, DEG C | 350 | 350 | 350 | 350 | 350 |
| Reaction pressure, MPa | 15 | 15 | 15 | 15 | 15 |
| Hydrogen to oil volume ratio | 1000:1 | 1000:1 | 1000:1 | 1000:1 | 1000:1 |
| Volume space velocity, h-1 | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 |
| Hydrogenation modifying process condition | |||||
| Reaction temperature, DEG C | 320 | 320 | 320 | 320 | |
| Reaction pressure, MPa | 15 | 15 | 15 | 15 | |
| Hydrogen to oil volume ratio | 1000:1 | 1000:1 | 1000:1 | 1000:1 | |
| Volume space velocity, h-1 | 1 | 1 | 1 | 1 | |
| Hydrogenation post-refining process condition | |||||
| Reaction temperature, DEG C | 180 | 180 | 180 | 180 | |
| Reaction pressure, MPa | 15 | 15 | 15 | 15 | |
| Hydrogen to oil volume ratio | 400:1 | 400:1 | 400:1 | 400:1 | |
| Volume space velocity, h-1 | 1 | 1 | 1 | 1 | |
| Purpose product yield, wt% | 85.2 | 85.2 | 85.2 | 92.1 | 87.1 |
3 product property of table
Coal direct liquefaction oil passes through hydrofinishing-hydro-upgrading-hydrofining it can be seen from embodiment 1-6
The physical property of the obtained transformer oil base oil of processing technology meet transformer oil standard, and index is preferable, illustrates the present invention
The feasible process with coal direct liquefaction oil processing transformer oil base oil proposed.
Only hydrofinishing does not have at hydro-upgrading process it can be seen from embodiment 1-6 and the product property of comparative example 1
The transformer oil base oil product that the coal direct liquefaction oil of reason obtains, anti-gassing property can be slightly good, but oxidation stability is poor, and
Electric property is bad (dielectric dissipation factor is high, and breakdown potential is forced down), and poor performance at low temperatures (- 38 DEG C), unqualified.
Coal direct liquefaction oil is by hydrofinishing-plus hydrogen it can be seen from embodiment 1-6 and the product property of comparative example 2
Modification-hydrofining three-level adds the transformer oil after hydrogen to decreased significantly than the condensed-nuclei aromatics content of comparative example 2, electrically
Performance also has a degree of promotion.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of transformer oil base oil, which is characterized in that the preparation method includes:
1) coal direct liquefaction oil is fractionated, obtains diesel oil distillate, the boiling range of the diesel oil distillate is 290~330 DEG C；
2) diesel oil distillate is subjected to hydrofining reaction, obtains hydrogenation products；
3) hydrogenation products are subjected to hydro-upgrading reaction, obtain the first transformer oil base oil；
4) first transformer oil base oil is subjected to hydrofining reaction, obtains the second transformer oil base oil；
Wherein the coal direct liquefaction oil includes oil A and oil B, wherein the volume ratio of the oil A and the oil B are 1:1~1:10,
Wherein the oil A described by weight percentage include 5%~15% alkane, 25%~35% cycloalkane, 50%~
60% mononuclear aromatics, 10%~20% double ring arene, 0%~10% thrcylic aromatic hydrocarbon, the sum of each component content are equal to
100%,
Wherein the oil B described by weight percentage include 0%~15% alkane, 5%~20% cycloalkane, 40%~
55% mononuclear aromatics, 35%~50% double ring arene, 5%~20% thrcylic aromatic hydrocarbon, the sum of each component content are equal to
100%.
2. preparation method according to claim 1, which is characterized in that the reaction of the hydrofining reaction in step 2)
Pressure is 3.0~21.0MPa, preferably 10.0~15.0MPa；Reaction temperature is 250~400 DEG C, preferably 300~350 DEG C；
The volume ratio of hydrogen and the diesel oil distillate is 400:1~2000:1, preferably 800:1~1200:1；Volume space velocity be 0.1~
2.5h-1, preferably 0.5~1.0h-1。
3. preparation method according to claim 1, which is characterized in that the reaction of the hydro-upgrading reaction in step 3)
Pressure is 3.0~21.0MPa, preferably 10.0~15.0MPa；Reaction temperature is 250~400 DEG C, preferably 300~340 DEG C；
The volume ratio of hydrogen and the hydrogenation products is 400:1~2000:1, preferably 800:1~1200:1；Volume space velocity be 0.1~
2.5h-1, preferably 0.8~1.5h-1。
4. preparation method according to claim 1, which is characterized in that the hydrofining in step 4) was reacted
Reaction pressure is 3.0~15.0MPa, preferably 6~15.0MPa；Reaction temperature be 140~300 DEG C, preferably 160~220
℃；The volume ratio of hydrogen and first transformer oil base oil is 200:1~2000:1, preferably 400:1~1000:1；Body
Product air speed is 0.1~2.5h-1, preferably 0.6~1.5h-1。
5. preparation method according to any one of claim 1 to 4, which is characterized in that the wherein oil A and oil B
Volume ratio be 1:2~1:8, preferably 1:3~1:7, more preferably 1:4~1:6, further preferably 1:6,
Preferably, the oil A described by weight percentage include 5%~10% alkane, 25%~30% cycloalkane, 50%
~55% mononuclear aromatics, 10%~15% double ring arene, 0%~5% thrcylic aromatic hydrocarbon, it is highly preferred that percentage by weight
The alkane for including 5%~7% than counting the oil A, 28%~30% cycloalkane, 50%~55% mononuclear aromatics, 10%
~15% double ring arene, 0%~2% thrcylic aromatic hydrocarbon,
Preferably, the oil B described by weight percentage include 0%~10% alkane, 5%~15% cycloalkane, 40%
~50% mononuclear aromatics, 35%~45% double ring arene, 5%~15% thrcylic aromatic hydrocarbon, it is highly preferred that percentage by weight
The alkane for including 0%~5% than counting the oil B, 5%~10% cycloalkane, 40%~45% mononuclear aromatics, 35%~
40% double ring arene, 5%~10% thrcylic aromatic hydrocarbon.
6. preparation method according to any one of claim 1 to 4, which is characterized in that in step 2), using adding hydrogen to protect
Protect catalyst and Hydrobon catalyst；Preferably, the filling of the hydrogenation protecting catalyst and the Hydrobon catalyst
Volume ratio is 1:2~1:6, preferably 1:4；Preferably, the hydrogenation protecting catalyst is RGC-1 series hydrogenation protecting catalyst
And/or FZC series hydrogenation protecting catalyst；Preferably, the hydrogenation protecting catalyst is to be with porous refractory inorganic oxide
The oxide of carrier, group VIB and/or group VIII metal is as active component, optionally containing the catalyst of P, Si, F, B；
Preferably, the Hydrobon catalyst is that RNC-2 series Hydrobon catalyst and/or FF-26 series hydrofinishing are catalyzed
Agent；Preferably, the active component of the Hydrobon catalyst is the oxide of group VIB and/or group VIII metal；It is preferred that
Ground, the Hydrobon catalyst described by weight percentage include 15~30% vib metals oxide；Preferably, it presses
Hydrobon catalyst described in weight percent meter includes 2~6% group VIII metal oxide；Preferably, described plus hydrogen
The specific surface of catalyst for refining is >=100m2/ g, pore volume are >=0.24ml/g.
7. preparation method according to any one of claim 1 to 4, which is characterized in that in step 3), using adding hydrogen to change
Matter catalyst；Preferably, the catalyst for hydro-upgrading is that RCC-1 series catalyst for hydro-upgrading and/or FC-28 series add hydrogen
Modifying catalyst；Preferably, the active component of the catalyst for hydro-upgrading is the oxygen of group VIB and/or group VIII metal
Compound；Preferably, the Hydrobon catalyst described by weight percentage includes 10~30% vib metals oxide；
Preferably, the Hydrobon catalyst described by weight percentage includes 4~10% group VIII metal oxide；It is preferred that
Ground, the specific surface area of the catalyst for hydro-upgrading are >=200m20.2~0.7mL/g of/g, Kong Rongwei, 3~10nm's of bore dia
Kong Rong accounts for the 70%~95% of total pore volume, preferably 85%~95%, and infrared acidity is 0.2~0.6mmol/g.
8. preparation method according to any one of claim 1 to 4, which is characterized in that in step 4), using adding hydrogen to mend
Fill catalyst for refining；Preferably, the hydrofining catalyst be RLF-20 series hydrofining catalyst and/or
FMTA-2 series hydrofining catalyst；Preferably, the active component of the hydrofining catalyst is Section VIII
The oxide of race's metal；Preferably, the hydrofining catalyst described by weight percentage includes the of 0.1%~2%
Group VIII metal oxide；Preferably, the hydrofining catalyst described by weight percentage includes 0.1%~0.8%
Pd oxide and 0.1%~0.5% Pt oxide；Preferably, the specific surface area of the hydrofining catalyst is
≥200m2/ g, Kong Rongwei >=0.5mL/g, bore dia are >=8nm, active metal H2Adsorbance is >=80mL/g.
9. a kind of transformer oil base oil of method preparation described in any item of the claim 1 to 8.
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