CN103666554B - A kind of hydroprocessing process producing high-quality solvent oil - Google Patents
A kind of hydroprocessing process producing high-quality solvent oil Download PDFInfo
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Abstract
A kind of hydroprocessing process producing high-quality solvent oil, kerosene(oil)fraction or solar oil feedstock oil-hydrogen mixture contact with non-noble metal hydrogenation process catalyst I in the first reaction zone and react, the effluent of the first reaction zone enters second reaction zone, with hydrogen counter current contact, and under the effect of non-noble metal hydrogenation process catalyst I I and noble metal hydrogenation catalyst for refining, carry out de-arylation reaction successively, wherein the temperature of reaction of second reaction zone is lower than the temperature of reaction of the first reaction zone 50 ~ 200 DEG C.Use method provided by the invention, can process kerosene or the solar oil cut of high sulfur-bearing, produce sulphur content and be less than 0.5 μ g/g, aromaticity content is less than the high-quality solvent product of 100 μ g/g.
Description
Technical field
The invention belongs to a kind of method of lower refining hydrocarbon ils in the presence of hydrogen, more particularly, is a kind of method of hydrotreating producing the extremely low food grade solvent oil of aromaticity content.
Background technology
In the deep-processing process of petroleum refining industry, kerosene(oil)fraction is widely used prospect.Kerosene raffinate cut can produce lam-oil, rocket engine fuel and all kinds of SOLVENTS oil production.The solvent oil product of solvent oil wherein, especially food grade has good price and outlet, is point of economic increase main in kerosene(oil)fraction post-treatment process.When producing solvent oil with kerosene feedstock, according to the needs in market, virgin kerosene can be carried out deep refining process, the aromaticity content of product is reduced to below certain requirement; Then be cut into narrow fraction product and be used as aerosol solvent, printing ink solvent, makeup tune and aluminium thin rolling wet goods product.
Traditional kerosene process for purification is clay-filtered method.But the quality product that the method obtains is low, and have that yield is low, equipment corrosion is serious and produce " " shortcoming such as many, is progressively eliminated the three wastes.
What current use was more is by Hydrofining Technology, obtains the solvent oil product that aromaticity content is qualified.Main technical process has: dewaxing by molecular sieve+solvent hydrogenation, high pressure single hop deep hydrogenation etc.But, adopt above-mentioned explained hereafter solvent oil to need to process raw material, and be difficult to realize producing the food grade solvent oil production that aromaticity content is 0.
US 5608025 discloses a kind of two-step approach aromatic saturation technique.Raw material successively through the reactor of two series connection, does not have separation facilities between reactor.Two-stage reaction is non-precious metal catalyst.When aromatics conversion rate is greater than 50%, reaction pressure need at more than 10.0MPa.
US 5183556 discloses a kind of diesel oil concurrent-countercurrent two sections of Porous deproteinized bone techniques.First paragraph adopts following current operation, adopts non-precious metal catalyst; Two sections adopt counter-current operation, adopt noble metal catalyst also can adopt non-precious metal catalyst.The clean diesel product of aromaticity content at 5 ~ 10v% can be produced.
US 5435907 discloses a kind of middle distillate deeply de-aromatizing method.Using a kind of take activated carbon as the catalyzer of carrier, processes the raw material of 160 ~ 250 DEG C, at 380 DEG C, under 10.8MPa and hydrogen to oil volume ratio are greater than the condition of 700Nm3/m3, aromaticity content 32% can be reduced to less than 10%.
EP 0699733 discloses a kind of diesel oil two sections of deeply de-aromatizing operating processes, and two sections adopt different operational conditions.First paragraph adopts non-precious metal catalyst, operates at relatively high temperature, the sulphur content of raw material is reduced to 500 below μ g/g; Second segment adopts noble metal catalyst to operate at relatively low temperatures, mainly completes aromatic saturation reaction.Air-lift device is had, to remove hydrogen sulfide and the ammonia of two section feedings between two-stage reaction.The diesel product adopting this patented technology can produce aromaticity content to be less than 20%.
Summary of the invention
The object of the invention is to provide a kind of method of hydrotreating producing the extremely low high-quality solvent oil of aromaticity content on the basis of existing technology.
Method provided by the invention is:
(1), after kerosene(oil)fraction or solar oil feedstock oil mix with hydrogen, its mixture enters the first reaction zone, contacts react with non-noble metal hydrogenation process catalyst I,
(2) effluent of the first reaction zone of step (1) gained enters second reaction zone, react with the hydrogen counter current contact entering second reaction zone, along the flow direction of the effluent of the first reaction zone, non-noble metal hydrogenation process catalyst I I and noble metal hydrogenation catalyst for refining is loaded successively in second reaction zone
(3) effluent of second reaction zone is after cooling, being separated, and obtains hydrogen-rich gas and solvent oil product,
Wherein the temperature of reaction of second reaction zone is lower than the temperature of reaction of the first reaction zone 50 ~ 200 DEG C, preferably 80 ~ 150 DEG C.
In the present invention, the boiling range of described kerosene(oil)fraction is 180 ~ 260 DEG C, and the boiling range of solar oil cut is 205 ~ 350 DEG C, can be kerosene(oil)fraction and the solar oil cut of different sources, is preferably virgin kerosene or straight distillation light diesel oil.
In a preferred embodiment in accordance with this invention, described second reaction zone is fixed-bed reactor, in reactor, from up to down load non-noble metal hydrogenation process catalyst I I and noble metal hydrogenation catalyst for refining successively, the reaction effluent of the first reactor enters fixed-bed reactor from top, hydrogen enters fixed-bed reactor from bottom, the overhead stream effluent of fixed-bed reactor is after cooling, being separated, the hydrogen-rich gas obtained recycles, and the liquid fraction of gained goes out device as hydrotreated naphtha product or boat coal blend component; The lower effluent of fixed-bed reactor, after being separated, obtains the solvent oil product that aromaticity content is extremely low.In addition, reverse-flow fixed-bed reactor have the effect of gas stripping column, the hydrogen sulfide in reaction product and ammonia can be removed, the reaction effluent of the first reaction zone is contacted with noble metal hydrogenation catalyst for refining in the reaction atmosphere that hydrogen sulfide is very low with ammonia density react, on the one hand, extend the activity stability time of noble metal hydrogenation catalyst for refining, on the other hand, be conducive to the carrying out of aromatic saturation reaction.At the top of fixed-bed reactor filling non-noble metal hydrogenation process catalyzer, be also in order to avoid hydrogen sulfide is to the Poisoning Effect of noble metal catalyst.
In the first reaction zone, kerosene(oil)fraction or solar oil feedstock oil-hydrogen mixture, contact with non-noble metal hydrogenation process catalyst I, at temperature of reaction 270 ~ 450 DEG C, hydrogen dividing potential drop 8.0 ~ 15.0MPa, hydrogen to oil volume ratio 60 ~ 1000Nm
3/ m
3, volume space velocity 1.0 ~ 3.0h
-1condition under, there is the reaction such as olefin saturation, hydrodenitrification reaction, hydrogenating desulfurization, aromatic saturation.
In second reaction zone, the reaction effluent of the first reactor is successively through non-noble metal hydrogenation process catalyst I I and noble metal hydrogenation catalyst for refining, and with hydrogen counter current contact, at temperature of reaction 200 ~ 320 DEG C, hydrogen dividing potential drop 8.0 ~ 15.0MPa, hydrogen to oil volume ratio 60 ~ 1000Nm
3/ m
3, volume space velocity 3.0 ~ 10.0h
-1condition under, carry out aromatic saturation reaction and product separation further.Because aromatic hydrogenation reaction exists thermodynamic(al)equilibrium restriction, high temperature can be unfavorable to aromatic hydrogenation saturated reaction.Therefore adopt relatively low temperature of reaction in second reaction zone, be conducive to the carrying out of the hydrotreated lube base oil reaction of aromatic hydrocarbons.
In second reaction zone, the admission space of non-noble metal hydrogenation process catalyst I I and noble metal hydrogenation catalyst for refining is than being 1:5 ~ 1:10.
Non-noble metal hydrogenation process catalyst I or non-noble metal hydrogenation process catalyst I I are loaded catalyst, and carrier is unformed aluminum oxide and/or sial, and active metal is be selected from one or more in VIB base metal and/or group VIII base metal.Wherein, group vib base metal is Mo and/or W, and group VIII base metal is Ni and/or Co.Non-noble metal hydrogenation process catalyst I and non-noble metal hydrogenation process catalyst I I can be identical catalyzer, also can be different catalyzer.
Preferred non-noble metal hydrogenation process catalyst I or non-noble metal hydrogenation process catalyst I I are for carrier with composite alumina and composite oxygen SiClx, it consists of: with oxide basis and with catalyzer total amount for benchmark, the content of nickel and/or cobalt is 2 ~ 8 heavy %, molybdenum and tungsten sum are 12 ~ 45 heavy %, and surplus is carrier.
Described noble metal hydrogenation catalyst for refining is loaded catalyst, carrier is heat-resistant inorganic oxide, load hydrogenation active component, described hydrogenation active component content, with oxide basis, be 0.01 ~ 15 heavy %, be selected from the mixture of one or more metals at least one platinum, palladium precious metal or itself and the group that is made up of molybdenum, nickel, vanadium, cobalt, tungsten.Preferred hydrogenation active component is the one combination in nickel-platinum, nickel-palladium, nickel-platinum-palladium, platinum-palladium.
When described hydrogenation active metals component is selected from the nickel of group VIII, platinum and/or metallic palladium component, be benchmark in metal and with catalyzer, the content of described group VIII metal is preferably 0.1 ~ 7 % by weight, and more preferably 0.1 ~ 5 % by weight.Time in described hydrogenation active metals component containing platinum and palladium, wherein Pd/(Pt+Pd) weight ratio be 0.3 ~ 1.0, preferably 0.5 ~ 0.8.
The optional self-alumina of described carrier, silicon oxide, titanium oxide, magnesium oxide, silica-alumina, alumina-silica magnesium, silica-magnesias, silica-zirconia, silica thoria, silica-berylias, silica-titania, silica-zirconia, titania-zirconia, silica-alumina thoria, silica-alumina-titania, silicaalumina-magnesia, silica-alumina, zirconia, natural zeolite, one or more in clay.Preferably aluminum oxide wherein and/or silica-alumina.
Described noble metal hydrogenation catalyst for refining can also contain selectable adjuvant component, and being one or more in boron, fluorine, chlorine and phosphorus, take catalyzer as benchmark, and the content of adjuvant component is 0.1% ~ 5.0 % by weight.
The invention has the advantages that:
1, use method provided by the invention, can process kerosene or the solar oil cut of high sulfur-bearing, produce sulphur content and be less than 0.5 μ g/g, aromaticity content is less than the high-quality solvent product of 100 μ g/g, and quality product reaches the requirement of food grade solvent oil.
2, in the present invention, the first reaction zone at high temperature operates, by sulfide most in raw material and organonitrogen removal, and saturated part aromatic hydrocarbons simultaneously; In the present invention, second reaction zone adopts adverse current bed bioreactor, have employed the noble metal catalyst that part aromatic saturation performance is good, and reacts under the operational condition being conducive to aromatic hydrogenation, can obtain better aromatic saturation effect.In addition, the top filling non-noble metal hydrogenation process catalyzer of the adverse current bed bioreactor in second reaction zone, avoids high density H
2s, to the influence of noble metal catalyst, extends the life cycle of noble metal hydrogenation catalyst for refining.
3, compared with two-stage hydrogenation, eliminate middle high pressure air lift facility, reduce equipment cost.
Accompanying drawing explanation
Accompanying drawing is the hydroprocessing process schematic flow sheet of production high-quality solvent oil provided by the invention.
Embodiment
Below by accompanying drawing, method provided by the invention is illustrated further, but not thereby limiting the invention.
The method of hydrotreating technical process of production high-quality solvent oil provided by the invention is described in detail as follows: new hydrogen enter make-up hydrogen compressor 19 boost after after pipeline 11 mixes with the recycle hydrogen from circulating hydrogen compressor 20, be divided into two-way, one tunnel mixes with fresh feed oil through pipeline 2, and another road enters the second reactor 15 through pipeline 4 bottom the second reactor 15.Fresh feed oil from pipeline 1 mixes with the hydrogen from pipeline 2, and mixing raw material enters the first reactor 14 and carries out hydrotreatment reaction.First reactor effluent of gained enters the second reactor 15 through pipeline 3 from the top of the second reactor, with the hydrogen counter current contact from pipeline 4, successively under the effect of non-noble metal hydrogenation process catalyst I I and noble metal hydrogenation catalyst for refining, remove the aromatic hydrocarbons in product further.Second hydrogenator 15 top material delivers to high-pressure separator 16 through pipeline 5, and separating obtained hydrogen-rich gas enters circulating hydrogen compressor 20 through pipeline 7, and separating obtained liquid product is extracted out through pipeline 8, as hydrotreated naphtha component.Second reactor 15 bottom material enters high-pressure separator 17 through pipeline 6, separating obtained gas is extracted out through pipeline 10, separating obtained liquid stream enters separation column 18 and cuts, and isolates lightnaphtha and extracts out through pipeline 12, isolates heavy naptha and extracts out through pipeline 13.
The following examples to method provided by the invention, will be further described, but not thereby limiting the invention.
Non-noble metal hydrogenation process catalyst I used in embodiment and non-noble metal hydrogenation process catalyst I I are Cat-A, and noble metal hydrogenation catalyst for refining is the trade names of Cat-B, Cat-A is RS-1000, is produced by Sinopec catalyzer branch office.The carrier of Cat-B is silica-alumina, take carrier as benchmark, and the content of its silicon oxide is 25 % by weight, and the specific surface area of carrier is 218m
2/ g, pore volume is 0.45ml/g; Active metal is Pt, Pd and Ni, take catalyzer as entirety, and the content of the content of Pt to be the content of 0.09 heavy %, Pd be 0.06 heavy %, Ni is 6 heavy %.
Stock oil A used in embodiment is a kind of virgin kerosene, and stock oil B is a kind of straight distillation light diesel oil.The main character of various raw material is as shown in table 1.
Aromatic hydrocarbons bioassay standard is SH/T 0415-92.
Embodiment 1
First stock oil A fully mixes with hydrogen, enters the first reaction zone, in high reaction temperatures, contacts carry out deep hydrodesulfurizationof reaction, denitrification reaction and part aromatic saturation and react with non-noble metal hydrogenation process catalyst I (Cat-A); Resultant of reaction enters second reaction zone, at non-noble metal hydrogenation process catalyst I I(Cat-A) and noble metal hydrogenation catalyst for refining (Cat-B) effect under, with hydrogen counter current contact, proceed the reaction of degree of depth aromatic saturation, the admission space of non-noble metal hydrogenation process catalyst I I and noble metal hydrogenation catalyst for refining is than being 1:7, meanwhile, the second reactor has the effect of gas stripping column, can remove the hydrogen sulfide in raw material and ammonia.Top, second reaction zone resultant of reaction is through cooling after being separated, and the hydrogen-rich gas of gained is recycle hydrogen, and the liquid fraction of gained goes out device as hydrotreated naphtha product or boat coal blend component; Bottoms directly enters fractionating system, isolates the solvent oil product of each fraction section.The reaction conditions of the present embodiment is as shown in table 2, and product main character is as shown in table 3, and as can be seen from Table 3, the aromaticity content of product is approximately 0, is the product index meeting food grade solvent oil.
Embodiment 2
First stock oil A fully mixes with hydrogen, enters the first reaction zone, contacts in high reaction temperatures to carry out deep hydrodesulfurizationof reaction, denitrification reaction and part aromatic saturation and react with non-noble metal hydrogenation process catalyst I (Cat-A); Resultant of reaction enters second reaction zone, at non-noble metal hydrogenation process catalyst I I(Cat-A) and noble metal hydrogenation catalyst for refining (Cat-B) effect under, with hydrogen counter current contact, proceed the reaction of degree of depth aromatic saturation, the admission space of non-noble metal hydrogenation process catalyst I I and noble metal hydrogenation catalyst for refining is than being 1:5.Meanwhile, the second reactor has the effect of gas stripping column, can remove the hydrogen sulfide in raw material and ammonia.Top, second reaction zone resultant of reaction is through cooling, and the hydrogen-rich gas of gained is recycle hydrogen, and the liquid fraction of gained goes out device as hydrotreated naphtha product or boat coal blend component; Bottoms directly enters fractionating system, isolates the solvent oil product of each fraction section.The reaction conditions of the present embodiment is as shown in table 2, and product main character is as shown in table 3, and as can be seen from Table 3, the aromaticity content of product is 30 μ g/g, is the product of high-quality solvent oil.
Table 1 stock oil character
| Stock oil is numbered | A | B |
| Type of feed | Virgin kerosene | Straight distillation light diesel oil |
| Density (20 DEG C), g/cm 3 | 0.805 | 0.823 |
| Sulphur content, μ g/g | 550 | 650 |
| Nitrogen content, μ g/g | 4.2 | 28 |
| Bromine valency, gBr/100g | 0.6 | 2.2 |
| Aromatic hydrocarbons, heavy % | 12.0 | 17.5 |
| Boiling range ASTM D-1160, DEG C | ||
| IBP | 185 | 208 |
| 10% | 208 | 228 |
| 50% | 225 | 275 |
| 90% | 243 | 303 |
| FBP | 255 | 333 |
Table 2 operational condition
| Numbering | Embodiment 1 | Embodiment 2 |
| Stock oil | A | B |
| First hydroconversion reaction zone | ||
| Hydrogen dividing potential drop, MPa | 10.0 | 12.0 |
| Temperature of reaction, DEG C | 300 | 320 |
| Volume space velocity during liquid, h -1 | 3.0 | 2.0 |
| Hydrogen to oil volume ratio, Nm 3/m 3 | 100 | 500 |
| Second hydroconversion reaction zone | ||
| Hydrogen dividing potential drop, MPa | 9.0 | 10.0 |
| Temperature of reaction, DEG C | 200 | 220 |
| Volume space velocity during liquid, h -1 | 1.5 | 1.3 |
| Hydrogen to oil volume ratio, Nm 3/m 3 | 100 | 300 |
Table 3 main products character
| Numbering | Embodiment 1 | Embodiment 2 |
| Sulphur content, μ g/g | <0.1 | <0.5 |
| Nitrogen content, μ g/g | <0.1 | <0.5 |
| Bromine valency, gBr/100g | <0.1 | <0.5 |
| Aromatic hydrocarbons, μ g/g | 0 | 30 |
| Boiling range scope ASTM D-1160, DEG C | 210～230 | 245～280 |
Claims (11)
1. produce a hydroprocessing process for high-quality solvent oil,
(1) kerosene(oil)fraction or solar oil feedstock oil mix with hydrogen, and its mixture enters the first reaction zone, contacts react with non-noble metal hydrogenation process catalyst I,
(2) effluent of the first reaction zone of step (1) gained enters second reaction zone, react with the hydrogen counter current contact entering second reaction zone, along the flow direction of the effluent of the first reaction zone, non-noble metal hydrogenation process catalyst I I and noble metal hydrogenation catalyst for refining is loaded successively, the reaction conditions of second reaction zone: temperature of reaction 200 ~ 320 DEG C, hydrogen dividing potential drop 8.0 ~ 15.0MPa, hydrogen to oil volume ratio 60 ~ 1000Nm in second reaction zone
3/ m
3, volume space velocity 3.0 ~ 10.0h
-1,
(3) effluent of second reaction zone is after cooling, being separated, and obtains hydrogen-rich gas and solvent oil product,
Wherein the temperature of reaction of second reaction zone is lower than the temperature of reaction of the first reaction zone 50 ~ 200 DEG C.
2. in accordance with the method for claim 1, it is characterized in that, the temperature of reaction of second reaction zone is lower than the temperature of reaction of the first reaction zone 80 ~ 150 DEG C.
3. in accordance with the method for claim 1, it is characterized in that, described second reaction zone is fixed-bed reactor, in reactor, from up to down load non-noble metal hydrogenation process catalyst I I and noble metal hydrogenation catalyst for refining successively, the reaction effluent of the first reactor enters fixed-bed reactor from top, hydrogen enters fixed-bed reactor from bottom, the overhead stream effluent of fixed-bed reactor is through cooling, after separation, the hydrogen-rich gas obtained recycles, the lower effluent of fixed-bed reactor is after being separated, obtain the solvent oil product that aromaticity content is extremely low.
4. in accordance with the method for claim 1, it is characterized in that, the reaction conditions of the first reaction zone: temperature of reaction 270 ~ 450 DEG C, hydrogen dividing potential drop 8.0 ~ 15.0MPa, hydrogen to oil volume ratio 60 ~ 1000Nm
3/ m
3, volume space velocity 1.0 ~ 3.0h
-1.
5. according to the method described in claim 1 or 3, it is characterized in that, in second reaction zone, the admission space of non-noble metal hydrogenation process catalyst I I and noble metal hydrogenation catalyst for refining is than being 1:5 ~ 1:10.
6. in accordance with the method for claim 1, it is characterized in that, non-noble metal hydrogenation process catalyst I or non-noble metal hydrogenation process catalyst I I are loaded catalyst, carrier is unformed aluminum oxide and/or sial, and active metal is be selected from one or more in VIB base metal and/or group VIII base metal.
7. in accordance with the method for claim 6, it is characterized in that, non-noble metal hydrogenation process catalyst I or non-noble metal hydrogenation process catalyst I I are for carrier with composite alumina and composite oxygen SiClx, it consists of: with oxide basis and with catalyzer total amount for benchmark, the content of nickel and/or cobalt is 2 ~ 8 heavy %, molybdenum and tungsten sum are 12 ~ 45 heavy %, and surplus is carrier.
8. in accordance with the method for claim 1, it is characterized in that, described precious metal catalyst for refining is loaded catalyst, carrier is heat-resistant inorganic oxide, load hydrogenation active component, described hydrogenation active component content, with oxide basis, be 0.01 ~ 15 heavy %, be selected from the mixture of one or more metals at least one platinum, palladium precious metal or itself and the group that is made up of molybdenum, nickel, vanadium, cobalt, tungsten.
9. in accordance with the method for claim 8, it is characterized in that, described hydrogenation active metals component is selected from the nickel of group VIII, platinum and/or metallic palladium component, and be benchmark in metal and with catalyzer, the content of described group VIII metal is 0.1 ~ 7 % by weight.
10. according to the method described in claim 8 or 9, it is characterized in that, containing platinum and palladium in described hydrogenation active metals component, wherein the weight ratio of Pd/ (Pt+Pd) is 0.3 ~ 1.0.
11. in accordance with the method for claim 1, it is characterized in that, the boiling range of described kerosene(oil)fraction is: 180 ~ 260 DEG C, is straight run kerosene fraction; The boiling range of described solar oil cut is: 205 ~ 350 DEG C, is straight distillation light diesel oil cut.
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| CN109423328A (en) * | 2017-08-24 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of method of solvent oil hydrogenation Porous deproteinized bone |
| CN111378502B (en) * | 2018-12-31 | 2021-12-07 | 中国石油化工股份有限公司 | Method for producing aromatic hydrocarbon solvent oil by hydrogenating C9 aromatic hydrocarbon fraction cracked by ethylene |
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| CN1157847A (en) * | 1996-12-26 | 1997-08-27 | 南京兴达石油化工科技工贸公司 | Method for producing special kerosene type solvent naphtha |
| CN1267709A (en) * | 1999-03-19 | 2000-09-27 | 中国石油化工集团公司 | Two-stage fraction oil hydrogenating and arene eliminating process |
| CN1488713A (en) * | 2002-10-10 | 2004-04-14 | 中国石油化工股份有限公司 | Hydrocarbon hdyrotreating method |
| CN102443431A (en) * | 2010-10-13 | 2012-05-09 | 天津河清化学工业有限公司 | Naphtha hydrorefining dearomatization method |
-
2012
- 2012-09-05 CN CN201210326384.7A patent/CN103666554B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1157847A (en) * | 1996-12-26 | 1997-08-27 | 南京兴达石油化工科技工贸公司 | Method for producing special kerosene type solvent naphtha |
| CN1267709A (en) * | 1999-03-19 | 2000-09-27 | 中国石油化工集团公司 | Two-stage fraction oil hydrogenating and arene eliminating process |
| CN1488713A (en) * | 2002-10-10 | 2004-04-14 | 中国石油化工股份有限公司 | Hydrocarbon hdyrotreating method |
| CN102443431A (en) * | 2010-10-13 | 2012-05-09 | 天津河清化学工业有限公司 | Naphtha hydrorefining dearomatization method |
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