CN101880549A - Hydrogenation method for liquefied gas fraction - Google Patents
Hydrogenation method for liquefied gas fraction Download PDFInfo
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- CN101880549A CN101880549A CN2009101359152A CN200910135915A CN101880549A CN 101880549 A CN101880549 A CN 101880549A CN 2009101359152 A CN2009101359152 A CN 2009101359152A CN 200910135915 A CN200910135915 A CN 200910135915A CN 101880549 A CN101880549 A CN 101880549A
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Abstract
The invention discloses a hydrogenation method for liquefied gas fraction, which is characterized by comprising the following steps of: filling at least one section of catalyst bed layer into a reactor, introducing a liquefied gas fraction raw material and hydrogen into the reactor from one or more sections of catalyst bed layers to contact a catalyst and perform hydrogenation saturation reaction, and reacting olefin in the liquefied gas fraction and the hydrogen to generate alkane and release a large amount of heat; after heat exchange, feeding the reaction product into a gas-liquid separator and separating the reaction product into a gas phase and a liquid phase, and introducing the separated gas phase flow into the reactor to perform repeated use; and introducing a part of separated liquid phase flow serving as a cyclic reaction product back to the reactor, and introducing the other part of the separated liquid phase flow serving as a liquefied gas fraction hydrogenation product out of the reactor to perform reuse. The hydrogenation product obtained by the method is saturated light hydrocarbon fraction which can be directly used as a raw material for an ethylene cracking device and also can be fractionated and cut into propane, n-butane and iso-butane and the like serving as high value-added chemical base raw materials so as to increase the economic benefit of an oil refining enterprise.
Description
Technical field
The invention belongs to a kind of hydrogenation saturation history of light hydrocarbons, specifically, is a kind of method of hydrotreating of liquefied gas fraction.
Background technology
Liquefied gas fraction mainly consist of C3, C4 alkane and alkene, also have a spot of C2 and C5 hydro carbons in addition.In the secondary processing process of oil product, all can produce liquefied gas fraction as technological processs such as thermally splitting, coking and catalytic cracking.Because cracking reaction is the process that is decomposed into the small molecules hydro carbons by macromolecule hydrocarbon, stable hydrocarbon generates stable hydrocarbon and alkene through the cracking reaction meeting, therefore, contains a large amount of alkene in the cracked reaction product, and the olefin(e) centent in the liquefied gas fraction is 10v%～80v%.
Liquefied gas fraction has following processing scheme usually after caustic wash desulfuration alcohol is handled: the first, and directly make civil liquefied gas and sell; Second, introducing gas fractionation plant separates according to each component boiling point difference, isolated propylene is as the raw material of devices such as polypropylene, vinyl cyanide or phenol-acetone, isolated iso-butylene is used for and the synthetic high octane value gasoline blending component MTBE of methyl alcohol reaction, and isolated butylene and Trimethylmethane are introduced alkyl plant and produced high octane value gasoline blending component through alkylated reaction; The 3rd, the liquefied gas fraction after desulfurization is handled is without fractionation, introduces polyunit and makes wherein alkene through the catalytic polymerization synthetic gasoline, and the propane and the butane of surplus are sold as motor liquified gas.The processing scheme of selecting liquefied gas fraction also will be considered the situations such as security of the advanced and operation of technology except needs are considered the situations such as supply and demand of the economic benefit of oil refining enterprise and produce market.More than in three kinds of schemes, propylene in the recovery liquefied gas makes the value-added process of product as the raw material and the iso-butylene of chemical plant installations through the synthetic MTBE of etherification reaction, and Trimethylmethane and butylene are subjected to the influence of liquefied gas and gasoline products price bigger through the process that alkylated reaction generates gasoline alkylate, when the close prices of liquefied gas and gasoline products, alkyl plant just is difficult to profitable, and the used catalyzer of alkyl plant is sulfuric acid or hydrofluoric acid, exist the hidden danger of safety and environmental protection, unless press for the clean gasoline component, just alkyl plant can be competitive.Domestic alkyl plant is subjected to economy and Influence on security majority to be in suspended state.In fact, the major part of liquefied gas fraction is still sold as civil liquefied gas.
Along with the progress of China at the natural gas exploration and development technical elements, gas production increases sharply and makes civil liquefied gas market be subjected to extruding, and in the competent area of natural gas supply, the civil liquefied gas price glides.Therefore, press for the application approach of further expansion liquefied gas fraction, to improve economic benefit of enterprises at these geographic oil refining enterprises of China.
Simultaneously, along with the development of chemical industry, the demand of China's ethene increases fast.The cracking of ethylene raw material that is used to produce ethene mainly contains ethane, propane, butane, petroleum naphtha, diesel oil and hydrocracking tail oil etc.Petroleum naphtha is main cracking of ethylene raw material, but is becoming tight the day of petroleum naphtha supply in recent years, and price rises steadily, and therefore, the raw material sources that enlarge ethylene cracker are necessary.
In the research in existing distillate hydrogenation field, do not see the report that the liquefied gas fraction hydrogenation is utilized again, this mainly is to be difficult to produce economic benefit to oil refining enterprise because the liquefied gas fraction hydrogenation utilizes again, olefin(e) centent in the liquefied gas fraction is than higher, in the hydrogenation saturation history, can consume a large amount of hydrogen, the price of hydrogen is considerably beyond the price of liquefied gas fraction, and the consumption of hydrogen accounts for the major part of liquefied gas fraction hydrogenation unit cost.In addition, liquefied gas fraction needs with special technique means control reaction heat because olefin(e) centent is higher, and the hydrogenation process liberated heat is more.Therefore, research institution studies fewerly to the hydrogen addition technology of liquefied gas fraction, does not see the report that complete set technology and products scheme are arranged.
Summary of the invention
The purpose of this invention is to provide the method that a kind of liquefied gas fraction hydrogenation utilizes again, to improve the economic benefit of oil refining enterprise processing liquefied gas fraction.
Method provided by the invention is: at least one section beds of filling in the reactor, liquefied gas fraction raw material and hydrogen through heat exchange reach reactor inlet temperature required after, introduce the reactor from one or more snippets beds upper space, contact with catalyzer, alkene in the liquefied gas fraction and hydrogen reaction generate alkane, and emit a large amount of heats, reaction product is after the heat exchange cooling, entering gas-liquid separator separates is gas-liquid two-phase, and isolated gaseous stream is introduced reactor and reused; An isolated liquid phase stream part is introduced reactor as the circulating reaction product, and another part utilizes as the liquefied gas fraction hydrogenation products again.
In the method provided by the invention, described liquefied gas fraction hydrogenation products is introduced ethane cracking furnace as the cracking of ethylene raw material, under 800～900 ℃ temperature, carry out scission reaction, reaction time is 0.1～0.5s, the product that the reaction back generates is introduced gas separation unit, isolate ethene, propylene and divinyl.
In the method provided by the invention, described liquefied gas fraction hydrogenation products is directly introduced gas separation unit, described gas separation unit is that a plurality of knockout towers are formed, and isolates propane, Trimethylmethane and normal butane, respectively as the Elementary Chemical Industry raw material.
In the method provided by the invention, described catalyzer is the base metal active ingredient that load is selected from VIB and/or VIII family on activated alumina or the amorphous silicon alumina supporter.
When containing diolefine in the described liquefied gas fraction raw material, the catalyzer of filling is preferably two kinds in the described reactor, upper strata filling selectivity is taken off the diene catalyzer, has lower reactive behavior, micro-diolefine in the selectivity saturated solution gasification feedstock, prevent from bed top very exothermic and quicken coke to generate, have higher voidage, avoid the beds pressure drop to increase fast; Lower floor's filling hydrocatalyst for saturating, the monoolefine in the saturated liquefied gas fraction.Two kinds of catalyzer all are to be prepared from activated alumina or amorphous silicon alumina supporter by the base metal active constituent loading that is selected from VIB and/or VIII family, just to take off diene activity of such catalysts component concentration lower slightly than hydrocatalyst for saturating for selectivity, and the admission space ratio of two kinds of catalyzer is (0.5～4.0): (9.5～6.0).Preferred selectivity is taken off the diene catalyzer and is consisted of, and is benchmark with the gross weight of catalyzer, contains the molybdenum oxide of 0.5～10.0w% nickel oxide and 3.0～35.0w%, and the alumina supporter of surplus; Consisting of of preferred hydrocatalyst for saturating is benchmark with the total catalyst weight, contains nickel oxide, 10～30w% Tungsten oxide 99.999 and the cobalt oxide 0.01～1.0w% of 1.0～7.0w%, and the alumina supporter of surplus.
In the method provided by the invention, the reaction conditions in the described hydrogenator is: temperature of reaction is 150～380 ℃, and the hydrogen dividing potential drop is 1.5～5.0MPa, and hydrogen to oil volume ratio is 100～600Nm
3/ m
3, the fresh feed volume space velocity is 1.0～6.0h
-1
The hydrogenation saturated reaction of the alkene in the liquefied gas fraction is a strong exothermal reaction, in hydrogenation process, for with the temperature rise control in the beds in the scope that requires, with the partial hydrogenation product as heating agent at the reactive system internal recycle, take away reaction heat, the weight ratio of circulating reaction logistics and fresh feed is (0.5～4.0): 1, preferred (1.0～2.0): 1.
In the method provided by the invention, described liquefied gas fraction raw material is C3, C4 hydro carbons and a spot of C2 and C5 hydrocarbon composition.Olefin(e) centent difference in the liquefied gas fraction that different raw materials or different oil product complete processings are produced is bigger, and the variation range of olefin(e) centent is 10.0～80.0v%.In order to adapt to the different alkene content in the liquefied gas fraction raw material, the invention provides the handiness of operation, when the olefin(e) centent in the raw material was low, the temperature rise in the reactor was less, can adopt less reaction product internal circulating load; When the olefin(e) centent in the raw material is higher, must be noted that the temperature rise in the controlling reactor, the method that can adopt has two kinds: the one, and the internal circulating load of raising reaction product recycle stream, make the olefin(e) centent of reactor inlet logistics be reduced to controlling valu, because it is controlled that the temperature rise in the increase of heating agent quantity, reactor relaxes; The 2nd, the hydrocatalyst for saturating bed in the reactor is divided into multistage or adopts a plurality of placed in-line reactors.
When the multistage hydrocatalyst for saturating bed that loads in the reactor, the liquefied gas fraction raw material is divided into multiply, wherein one mixes with reaction product recycle stream and recycle hydrogen, after being heated to reactor inlet temperature, introduced by reactor inlet, all the other each stocks are not introduced in the space between other adjacent two-stage catalytic agent beds, realize mending mixing and distribution of material and reactant flow in inner member, preferably the beds in the reactor is divided into 2～3 sections, reaction raw materials is divided into 2～3 strands.
In the method provided by the invention, described reactor can be made up of placed in-line two hydrogenators at least, preferred 2～3 reactors, described liquefied gas fraction raw material, circulating reaction product and hydrogen are divided into multiply, through heat exchange and be heated to reactor inlet temperature required after, introduce respectively in a plurality of hydrogenators, contact with beds and to carry out the hydrogenation saturated reaction, reacted product is introduced gas-liquid separator and is divided into gas-liquid two-phase, and isolated gaseous stream is introduced reactor and reused; An isolated liquid phase stream part is drawn back reactor as the circulating reaction product, and another part is drawn reactor as the liquefied gas fraction hydrogenation products and utilized.A kind of introducing mode is that one described liquefied gas raw material is wherein mixed with reaction product recycle stream and recycle hydrogen, after being heated to reactor inlet temperature, introduce by reactor inlet, all the other each strand liquefied gas raw materials are introduced respectively in the pipeline between other adjacent two reactors, and enter next reactor after reactant flow is mixed.
Introducing reaction raw materials between adjacent two beds or between adjacent two reactors, olefin saturation is effectively controlled, bring into play the effect of bed inner catalyst better, can also play the effect of cold shock medium, the medial temperature of control bed can play the effect that reduces the reaction product internal circulating load in addition.
Method provided by the invention has following beneficial effect:
(1) adopts method treatment solution gasification cut provided by the invention, obtain the hydrogenation products of saturated light ends fractionation.Described hydrogenation products can be directly as the raw material of ethylene cracker, because carbochain is short and contain more normal paraffin, the yield of ethene height is the cracking of ethylene raw material that is better than petroleum naphtha and heavy distillate, has enlarged the raw material sources of ethylene cracker; Described hydrogenation products can also be cut into different components by fractionating method, as propane, normal butane and Trimethylmethane etc., sells as the industrial chemicals that added value is higher, further expands the application approach of liquefied gas fraction, increases the economic benefit of oil refining enterprise.
(2) method provided by the invention need be by the alkene in the saturated liquefied gas fraction of hydrogenation reaction, and the hydrogenation saturated reaction of alkene is a strong exothermal reaction, the present invention is by adopting the partial reaction product at the reactive system internal recycle, make the reaction liberated heat in time shift out reactor, the temperature rise of beds is effectively controlled, and can avoid the appearance of temperature runaway phenomenon in the hydrogenator.
(3) preferred version of method provided by the invention can be divided into multiply with the liquefied gas fraction raw material, except that the inlet that has one from reactor is introduced, all the other each strand raw materials are introduced respectively in the same reactor in the space between adjacent two beds, or introduce in the pipeline between adjacent two reactors of placed in-line a plurality of reactors.The share split of liquefied gas fraction raw material is introduced can make the easier control of olefin hydrogenation, the introducing raw material that temperature is lower can also play the effect of cold shock medium, be used for the temperature of reaction of different axial locations in the conditioned reaction device, thereby can reduce the internal circulating load of reaction product recycle stream, save the power consumption of recycle pump.
Description of drawings
Accompanying drawing is the process flow diagram of liquefied gas fraction method of hydrotreating provided by the invention.
Embodiment
Below in conjunction with accompanying drawing liquefied gas fraction method of hydrotreating provided by the present invention is further detailed, but not thereby limiting the invention.
The technical process of this method is as follows: the liquefied gas fraction raw material enters fresh feed pump 2 through pipeline 1, by being divided into two strands after fresh feed pump 2 superchargings, wherein one raw material is via between the two-stage catalytic agent bed in the pipeline 4 introducing reactors 10, play cold shock medium and control reaction depth, after another strand raw material mixes via the recycle hydrogen of the circulating reaction logistics of pipeline 3 and pipeline 21 and pipeline 26, enter into/effluent exchanger 6 through pipeline 5, after the reaction product heat exchange, enter charging process furnace 8 through pipeline 7, it is temperature required after enter reactor 10 by pipeline 9 that mixture flow is heated to reactor inlet.Beds in the reactor 10 is divided into two sections, the top of epimere beds is filled with selectivity and takes off the diene catalyzer, hydrocatalyst for saturating is equipped with in the bottom, the lower section catalyst bed also is filled with selectivity and takes off the diene catalyzer on top, hydrocatalyst for saturating is equipped with in the bottom, be provided with inner member in the space between two-stage catalytic agent bed, the liquefied gas fraction raw material that the reactant flow of the heat that the upper catalyst bed layer comes and the temperature of pipeline 4 introductions are lower mixes in inner member, and be evenly distributed to the top of lower catalytic agent with desired temperature, in the lower catalyst bed layer, proceed the hydrogenation saturated reaction of alkene.Reactant flow is drawn reactor 10 by pipeline 11, successively through advancing/effluent exchanger 6, air cooler 13, water cooler 15 enter gas-liquid separator 17.The gaseous stream of gas-liquid separator 17 is drawn by pipeline 22, after compressed machine inlet buffer 23 is told a small amount of lime set, enter circulating hydrogen compressor 25 by pipeline 24, recycle hydrogen after the supercharging is drawn by pipeline 26, hydrogen make-up is by pipeline 27 drawing-in systems, and by after new hydrogen supercharger 28 superchargings, mix through the recycle hydrogen of pipeline 29 with pipeline 26, mixed mixing hydrogen mixes with liquefied gas fraction raw material and circulating reaction product in the pipeline 3 again, provide hydrogenation reaction required hydrogen, and guard catalyst plays the effect that reduces carbon deposit; After being drawn by container bottom, the liquid phase stream of gas-liquid separator 17 is divided into two strands, wherein one via pipeline 19 by 20 superchargings of reaction product recycle pump after, mix via the liquefied gas fraction raw material in pipeline 21 and the pipeline 3, as heating agent at system's internal recycle, another strand drawn by pipeline 18 as hydrogenation products, can hydrogenation products be separated into required component with fractionated method according to different requirements to the purpose product.
Present embodiment will give further instruction to practical situations of the present invention, and this is a special case of the present invention, and is not thereby limiting the invention.
Embodiment
The technical process that the liquefied gas fraction raw material of embodiment adds hydrogen partial as shown in drawings, the liquefied gas fraction raw material mixes with circulating reaction product and recycle hydrogen respectively, after heat exchange and heating, enters hydrogenator.The filling selectivity is taken off diene catalyzer (trade names are RGO-2) and hydrocatalyst for saturating (trade names are RS-1) in the hydrogenator, and the admission space ratio of the two is 2: 8.RGO-2 and RS-1 produce by catalyzer Chang Ling branch office of China Petrochemical Corp..The partial hydrogenation reaction product is drawn reaction unit introduce ethane cracking furnace, as the raw material of ethylene cracker.The composition of liquefied gas fraction raw material sees Table 1, hydrogen is formed and seen Table 2, and hydrogenation conditions, hydrogenation products are formed, ethane cracking furnace reaction conditions and split product are formed and seen Table 3.
Table 1 liquefied gas fraction raw material is formed
| Component | Content, v% |
| Normal butane | ??19.62 |
| Component | Content, v% |
| Trimethylmethane | ??36.29 |
| N-butene | ??10.39 |
| Iso-butylene | ??19.19 |
| Along 2-butylene | ??5.91 |
| Anti-2-butylene | ??8.06 |
| Divinyl | ??0.54 |
| Amount to | ??100 |
Table 2 hydrogen is formed
| Component | Content, v% |
| Hydrogen | ??92.3 |
| C1～C4 hydro carbons | ??7.7 |
By table 1, table 2 as seen, the liquefied gas fraction raw material of embodiment serves as main the composition with the C4 hydrocarbon, and its olefin(e) centent is 44.09 volume %, and hydrogen make-up is the hydrogen of catalytic reforming unit by-product, and its hydrogen content is 92.3v%.
Table 3
By table 3 as seen, for control reaction temperature, the flow of circulating reaction product is 1.5: 1 with liquefied gas fraction raw material weight ratio.The liquefied gas fraction raw material is behind hydrogenation, and the saturated alkane that generated of hydrogenation of olefins has only normal butane and Trimethylmethane in the hydrogenation products.With the liquefied gas fraction hydrogenation products as the cracking of ethylene raw material, under the condition of 850 ℃ of cracking temperatures and residence time 0.15s, carry out scission reaction, yield of ethene has reached 40.3w%, and the ethylene yield when being cracking stock far above petroleum naphtha or diesel oil (25w%～35w%).
Claims (10)
1. the method for hydrotreating of a liquefied gas fraction, it is characterized in that at least one section beds of filling in the reactor, liquefied gas fraction raw material and hydrogen are introduced the reactor from one or more snippets beds, contact with catalyzer and to carry out the hydrogenation saturated reaction, alkene in the liquefied gas fraction and hydrogen reaction generate alkane, and emit a large amount of heats, and reaction product is after heat exchange, enter gas-liquid separator and be divided into gas-liquid two-phase, isolated gaseous stream is introduced reactor and is reused; An isolated liquid phase stream part is drawn back reactor as the circulating reaction product, and another part is drawn reactor as the liquefied gas fraction hydrogenation products and utilized.
2. according to the method for claim 1, it is characterized in that described liquefied gas fraction hydrogenation products as carrying out scission reaction in the cracking of ethylene raw material introducing ethane cracking furnace, cracking temperature is 800-900 ℃, the residence time is 0.1-0.5s, the product that generates is introduced gas separation unit, obtain ethene, propylene and divinyl.
3. according to the method for claim 1, it is characterized in that described liquefied gas fraction hydrogenation products is introduced gas separation unit, isolate propane, Trimethylmethane and normal butane, and respectively as the Elementary Chemical Industry raw material.
4. according to claim 1,2 or 3 method, it is characterized in that described catalyzer is to be selected from the base metal active constituent loading of VIB and/or VIII family on activated alumina or amorphous silicon alumina supporter.
5. according to claim 1,2 or 3 method, the catalyzer that it is characterized in that described catalyst in reactor bed filling is two kinds, beds upper strata filling selectivity is taken off the diene catalyzer, beds lower floor filling hydrocatalyst for saturating, described selectivity takes off the diene catalyzer and hydrocatalyst for saturating all is to be prepared from activated alumina or amorphous silicon alumina supporter by the base metal active constituent loading that is selected from VIB and/or VIII family, and the admission space ratio of two kinds of catalyzer is (0.5～4): (9.5～6).
6. according to the method for claim 5, it is characterized in that described selectivity takes off the diene catalyzer and consist of, be benchmark with the gross weight of catalyzer, contain the nickel oxide of 0.5～10.0w% and the molybdenum oxide of 3～35w%, and the alumina supporter of surplus; Consisting of of described hydrocatalyst for saturating is benchmark with the total catalyst weight, contains the nickel oxide of 1.0～7.0w%, Tungsten oxide 99.999 and the 0.01～1.0w% cobalt oxide of 10～30w%, and the alumina supporter of surplus.
7. according to claim 1,2 or 3 method, it is characterized in that the reaction conditions in the described hydrogenator is: temperature of reaction is 150～380 ℃, and the hydrogen dividing potential drop is 1.5～5.0MPa, and hydrogen to oil volume ratio is 100～600Nm
3/ m
3, the fresh feed volume space velocity is 1.0～6.0h
-1
8. according to claim 1,2 or 3 method, it is characterized in that the weight ratio of described circulating reaction product and liquefied gas fraction raw material is (0.5～4.0): 1.
9. according to the method for claim 8, it is characterized in that the weight ratio of described circulating reaction product and liquefied gas fraction raw material is (1.0～2.0): 1.
10. in accordance with the method for claim 1, it is characterized in that described reactor is made up of placed in-line two hydrogenators at least, described liquefied gas fraction raw material, circulating reaction product and hydrogen are divided into multiply, through heat exchange and be heated to reactor inlet temperature required after, introduce respectively in a plurality of hydrogenators, contact with beds and to carry out the hydrogenation saturated reaction, reacted product is introduced gas-liquid separator and is divided into gas-liquid two-phase, and isolated gaseous stream is introduced reactor and reused; An isolated liquid phase stream part is drawn back reactor as the circulating reaction product, and another part is drawn reactor as the liquefied gas fraction hydrogenation products and utilized.
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| WO2023220167A1 (en) * | 2022-05-12 | 2023-11-16 | Lummus Technology Llc | Production of heavy isoparaffinic hydrocarbons |
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