CN1854264A - Integrated Fischer-Tropsch synthetic oil hydrogenation purification - Google Patents
Integrated Fischer-Tropsch synthetic oil hydrogenation purification Download PDFInfo
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Abstract
A kind of integrated hydrogenation improving quality method for the oil fractions from Fishcher-Tropsch synthesis process, it is used to gain high quality middle fraction oil. The all fractions and hydrogen contact with hydrofining catalyst, the middle fraction oil gained after isolation, naphtha and tail oil will be mixed by the reactant liquor of hydrofining and the reactant liquor of hydrocracking reactant liquor, the tail oil and hydrogen will be mixed and then circulate to isocracking reacktor and contact with hydrocracking and isocracking catalyst. The yield of the diesel oil is higher than 80% by the method, and the cetane number will be as high as 80, The water produced by hydrofining process can be prevented to go into the isocracking reacktor by this method, the availability and using periodic can also be improved. Moreover, the technological process of this method is high integrated; the equipment needed is fewer, so the cost of investment and operation can be decreased.
Description
Technical field
The invention belongs to a plurality of hydrogenation processes of a kind of usefulness and handle the method for hydrocarbon ils, more particularly, being hydroprocessing technique of a kind of usefulness and one exists cracking process under the situation of hydrogen to handle the method for Fischer-Tropsch synthesis oil.
Technical background
The employed fuel main source of the various vehicles is an oil on the our times, and the various derivatives of oil provide powerful motivation for development economic and society.But oil is as the non-renewable energy; be faced with exhausted day by day crisis; and; the quality of crude oil also worse and worse; undesirable components content such as condensed-nuclei aromatics, sulphur, nitrogen increase day by day in the composition of its derivative; cause the course of processing that before becoming the fuel commodity, needs through increasingly sophisticated, remove the component that influences environment, cause the process for processing cost significantly to increase.Therefore, need to seek alternative fuel to solve energy problem.
Coal or Sweet natural gas etc. comprise through the production technique principle process of oil from Fischer-Tropsch synthesis: coal or gas material are converted into hydro carbons and synthetic oil processing such as straight-chain paraffin, alkene through gasification generation raw gas, refining synthetic gas, the synthetic gas of obtaining of raw gas purifying through the Fischer-Tropsch building-up reactions.
Just with impurity removals such as sulphur, nitrogen, this following process to product is very favourable on the source for the production purifying step of synthetic gas (being made up of hydrogen and carbon monoxide); Fischer-Tropsch synthesis is to be raw material with the synthetic gas, generates the reaction of hydro carbons under the synthetic catalyst effect, has in synthetic gas wide material sources, the product advantages such as undesirable components content such as sulphur, nitrogen, aromatic hydrocarbons are low.The synthetic oil that adopts the Fischer-Tropsch synthetic technology to obtain, comparing with the conventional oil derivative in each side such as hydrocarbon composition and main character has bigger difference, is a kind of material of high content of wax composition, mainly be made of alkane and alkene, and sulphur, nitrogen content is very low.
Because the introducing of oxygen has determined wherein to contain a certain amount of oxygenatedchemicals in its synthetic gas production process, as alcohol, acid etc., can a certain amount of water of generation in the follow-up course of processing, can produce adverse influence to the use of catalyzer; The olefin(e) centent height is because the reaction mechanism of this production process is produced alkane by generating the alkene intermediate product.Oxidation not only himself takes place and superimposedly waits reaction in the existence of a large amount of alkene easily, but also can promote the oxidizing reaction of other hydro carbons, and generation has a strong impact on the products such as colloid of oil product use properties.Fischer-Tropsch synthesis oil need pass through corresponding hydrogenation upgrading, just can obtain meeting the liquid fuel that uses specification.
US2003/0057135A1 discloses a kind of method that adopts hydroisomerizing/hydrocracking process to be generated oily production middle runnings by Fischer-Tropsch synthesis, this method is cut into two cuts of weight with the Fischer-Tropsch synthesis product, cut point is about 150 ℃, and＜150 ℃ lighting end devaporation cracker is as the raw material of producing alkene;＞150 ℃ last running is earlier through hydrotreating step, and hydrogenation is removed unsaturated hydro carbons such as alkene and oxygenatedchemicals etc.; Logistics after the hydrotreatment enters the hydroisomerizing cracking case after passing through the step that dewaters, the hydroisomerizing cracking catalyst is a noble metal catalyst, carrier is an amorphous aluminum silicide, last running generation hydroisomerization and hydroisomerizing cracking reaction, reacted product enters separation column cutting and obtains each cut, and＞370 ℃ of cuts loop back hydrocracking reactor.This method has increased the step that dewaters, and make technical process complicated, and the intermediate oil yield is lower.
It is raw material is produced intermediate oil by hydrocracking and hydroisomerisation process method with the Fischer-Tropsch synthetic that US5378348 discloses a kind of, this method is by being divided into the Fischer-Tropsch synthesis product petroleum naphtha (C5-160 ℃), lighting end (160-260 ℃) and three cuts of last running (＞260 ℃), hydrocracking reaction is carried out in＞260 ℃ last running, and unconverted＞370 a ℃ heavy ends loops back hydrocracking reactor and continues cracking.Catalyst system therefor is noble metal catalyst or Ni+Co/Mo catalyzer, and transformation efficiency is controlled at the heavy % of 39-53; Lighting end with carry out hydrotreatment after the light constituent product that hydrocracking reaction obtains mixes olefin saturation and hydrogenation deoxidation reaction mainly take place, kerosene carries out hygrogenating isomerization reaction then, improves the different direct ratio (ratio of isomery hydro carbons and positive structure hydro carbons) in the hydrocarbon composition.This method can increase the productive rate of distillates such as kerosene, diesel oil, and these products have good low temperature flowability, and the kerosene freezing point can reach-43 ℃, and diesel oil (260-370 ℃) pour point can reach about 27 ℃.Because this method has increased isomerization-visbreaking catalytic reaction process and separation column, make its technical process comparatively complicated; Increased the isomerization-visbreaking section, catalyst levels also significantly increases; Unifining process generates water and directly enters into the isomerization-visbreaking reactor, for the isomerization-visbreaking catalyzer certain influence is arranged; The intermediate oil yield is not high yet.
US6309432 discloses a kind of method of producing rocket engine fuel from Fischer-Tropsch synthesis oil, this method is cut into two cuts of weight with Fischer-Tropsch synthesis oil earlier under 371 ℃,＜371 ℃ lighting end successively separates with cold branch through overheated branch and obtains 246 ℃ of-371 ℃ of cuts and C5-246 ℃ of cut, 246 ℃ of-371 ℃ of cuts and＞371 ℃ of last running are through the hydroisomerizing cracking case, saturated at alkene, in the time of the oxygenatedchemicals hydrogenation, normal paraffin generation hydroisomerizing and hydrocracking reaction, isomerized products is mainly monomethyl branching hydro carbons, and cracking conversion rate is about 30-50%; C5-246 ℃ of cut is without hydrotreatment, to keep oxygenatedchemicals wherein to the effect of being significantly improved of rocket engine fuel lubricity, it mainly is C7-C12 straight chain alcohols, remove separation column after this cut and hydrocracking reactor product are mixed together, cutting obtains cuts such as corresponding rocket engine fuel.Owing to contain the alkene and the nitrogen content of high level in the Fischer-Tropsch oil, directly contact with the isocracking catalyzer, stable and disadvantageous effect is arranged running period to it, and quality product is relatively poor.
Summary of the invention
The objective of the invention is to provide on the basis of existing technology a kind of Fischer-Tropsch synthetic oil hydrogenation purification, obtain high-quality middle runnings oil production with maximum.
Method provided by the invention comprises:
The full cut of Fischer-Tropsch synthesis oil, hydrogen contact with Hydrobon catalyst, hydrofining reaction logistics and hydrocracking reaction logistics mix through separating and obtain intermediate oil product and petroleum naphtha and tail oil, are circulated to the isocracking reactor after tail oil and the hydrogen mixing and contact with the hydroisomerizing cracking catalyst.
This method diesel product yield is higher than 80 heavy %, and its cetane value is up to 80, and the water of having avoided unifining process to generate enters into the isocracking reactor, improves the utilization ratio and the life cycle of catalyzer.In addition, this method flow height is integrated, equipment is few, can reduce investment and process cost.
Description of drawings
Accompanying drawing is an integrated Fischer-Tropsch synthetic oil hydrogenation purification schematic flow sheet provided by the present invention.
Embodiment
Distinguishing feature of the present invention is the technical process of having adopted integrated form.
Method provided by the invention is so concrete enforcement:
For prevent that the alkene in the Fischer-Tropsch synthesis oil from reactions such as polymerization taking place in the following process process, the full cut of Fischer-Tropsch synthesis oil, hydrogen enter hydrofining reactor, and reactions such as hydrogenation deoxidation, alkene be saturated take place under the Hydrobon catalyst effect.Synthetic oil after the hydrofining is successively after high and low pressure separates, enter separation column cutting, after cutting out light, heavy naphtha and coal, diesel oil distillate, the tail oil that obtains at the bottom of the separation column enters hydrocracking reactor, under the effect of hydroisomerizing cracking catalyst, heavy ends is converted into the intermediate oil product to greatest extent.The reaction product of hydrocracking reactor and hydrofining reaction product mix successively after high and low pressure separates, and enter separation column cutting and obtain the purpose product.
Synthetic oil after the hydrofining cuts out heavy ends (as boiling point＞370 ℃) through separation column, and this heavy ends enters the cracking reaction of hydrocracking reactor generation hydroisomerizing.Like this, do not enter hydrocracking reactor, reduced the volume and the catalyst levels of hydrocracking reactor on the one hand, thereby reduced facility investment, running expense and catalyst costs through the light ends after the hydrofining; Also reduced lighting end on the other hand the generation that overcracking reacts has taken place under the hydrocracking catalyst effect, reduce the generation of gaseous product and small molecules undesirable components, guaranteed the yield of ideal composition such as middle runningss such as rocket engine fuel, diesel oil to greatest extent.
After the hydrofining of Fischer-Tropsch synthesis oil raw material with hydroisomerizing cracking catalyst contact reacts, alkene and close catalyst activity that a large amount of coke that generation vigorous reaction such as oxygen compound generates the cause phenomenon that descends rapidly when having avoided the hydroisomerizing cracking catalyst and hydrofined oil directly not contacting has prolonged the running period of catalyzer.The present invention has also avoided unifining process to generate water and has entered into the isocracking reactor, can improve the utilization ratio and the life cycle of catalyzer.
Since during the Fischer-Tropsch synthetic hydro carbons constitutes based on positive structure hydro carbons, the isomery hydro carbons changed very little with the ratio (hereinafter to be referred as different direct ratio) of positive structure hydro carbons during the hydro carbons of the naphtha fraction that naphtha fraction in the raw material and hydrofining generate constituted, if used as the gasoline blend component, its octane value is lower.For addressing the above problem, when being productive target with the gasoline blending component, establish a heterogeneous catalyst bed in the hydrofining reactor bottom among the present invention, utilize hydroisomerisation catalysts, improve the different direct ratio in each cut hydro carbons formation refining reaction product generation isomerization reaction.
In hydrocracking reactor, for to greatest extent the heavy hydrocarbon highly selective being converted into particularly diesel oil distillate of middle runnings oil production, adopt the hydroisomerizing cracking catalyst, the control transformation efficiency reaches higher level at the preferred 40%-60% of 30%-80% to guarantee the selectivity that diesel oil distillate generates; Strengthen hygrogenating isomerization reaction simultaneously, make that the different direct ratio in the purpose product significantly improves, guaranteeing the low-temperature performance of purpose product, can meet the requirement of currently available products standard as the character such as condensation point of the freezing point of boat coal and diesel oil.
In the present invention, hydrofining reaction route and hydrocracking reaction route common high voltage separator, light pressure separator and separation column, thus saved facility investment greatly.Substantially do not contain sulphur, nitrogen in the Fischer-Tropsch synthesis oil, therefore react and also do not contain gases such as hydrogen sulfide and ammonia in the gas phase substantially, and because hydrofining reaction relatively easily carries out, the hydrogen consumption is low, so the hydrogen-containing gas that high-pressure separator obtains can directly be originated as hydrofining reaction hydrogen.
In the present invention, hydrogenation reaction is to carry out under hydrogen dividing potential drop 2.0-16.0MPa, 250-430 ℃ of hydrofining reaction temperature, and hydroisomerizing cracking reaction temperature is 300-450 ℃, cumulative volume air speed 0.1-4.0h
-1, hydrogen to oil volume ratio 100-1500v/v.
In the present invention, used Hydrobon catalyst is a kind of metal load type catalyst, and carrier is unformed aluminum oxide, and metal component is VIB or/and VIII family base metal, and wherein the group vib metal is Mo or/and W, and VIII family metal is that Co is or/and Ni.
In the present invention, used hydroisomerizing hydrocracking catalyst is the noble metal catalyst or the non-precious metal catalyst of amorphous aluminum silicide load.The metal component of non-precious metal catalyst is VIB or/and VIII family base metal, and wherein the group vib metal is Mo or/and W, and VIII family metal is that Co is or/and Ni; The metal component of noble metal catalyst is that Pt is or/and Pd.
Because the olefin(e) centent in the coal Fischer-Tropsch synthesis oil is very high,, can on catalyzer, generate a large amount of coke and cause catalyst activity reduction by vigorous reaction if alkene is direct and the Hydrobon catalyst contact reacts; Generally contain a certain amount of metal in the Fischer-Tropsch synthesis oil; these metals very easily are deposited on the Hydrobon catalyst top; cause reactor pressure reduction to occur; be deposited on metal on the catalyzer simultaneously and can cause the permanent deactivation of hydrogenation catalyst; for guaranteeing the long-term operation of full scale plant; preferably the hydrogenation protecting agent is seated in the Hydrobon catalyst top, thereby avoids the generation of above-mentioned phenomenon.Described protective material is to load on VIB on unformed aluminum oxide or the silica-alumina supports or/and VIII family non-precious metal catalyst, and wherein the group vib metal is Mo or/and W, and VIII family metal is Co or/and Ni, and this protective material has bigger pore volume and specific surface area.The volume ratio of protective material and Hydrobon catalyst is 0-30: 100 preferred 5-20: 100.
In addition, because the isomery hydrocracking reaction has a spot of alkene to generate, for guaranteeing constant product quality, should load a spot of back catalyst for refining in the bottom of isomery hydrocracking reactor, the volume ratio of back finishing agent and isocracking catalyzer is 0-15: 100 preferred 5-10: 100.
Below in conjunction with accompanying drawing method provided by the present invention is further detailed.
Accompanying drawing is an integrated Fischer-Tropsch synthetic oil hydrogenation purification schematic flow sheet provided by the present invention, has omitted equipment such as process furnace, interchanger, pump and valve among the figure.
This flow process describes in detail as follows: the coal synthetic gas after the purification enters 17 reactions of Fischer-Tropsch synthesis device through pipeline 1; the Fischer-Tropsch synthesis oil that obtains through pipeline 2 with enter hydrofining reactor 18 after hydrogen-rich gas from pipeline 16 mixes; successively with hydrogenation protecting agent, Hydrobon catalyst contact reacts; remove oxygen, metal impurities in the oil on the one hand, make a large amount of alkene generation saturated reactions in the oil on the other hand.Waiting hydrofining reaction owing to alkene is saturated is strong exothermal reaction, so there is cold hydrogen to inject between each beds of refining reaction device, with control reaction temperature, prevents out of control situation generations such as overtemperature.The effluent of hydrofining reactor 17 is through pipeline 3 and the logistics that obtains after hydrocracking reaction product from pipeline 4 mixes, enter high-pressure separator 20 through pipeline 5, in high-pressure separator 20, be separated into two bursts of logistics, wherein one is a hydrogen-rich stream, its composition is mainly hydrogen, this logistics after new hydrogen from make-up hydrogen compressor 24 mixes, loops back hydrocracking reactor 19, hydrofining reactor 18 through pipeline 15,16 respectively after pipeline 7 enters circulating hydrogen compressor 23 compression; Another burst logistics of high-pressure separator 20 enters light pressure separator 21 through pipeline 6, further remove lightweight small molecules hydro carbons, light pressure separator 21 bottom effluents enter fractionating column system 22 through pipeline 8, fractionate out gaseous product, naphtha fraction, the rocket engine fuel cut, diesel oil distillate and tail oil cut, gaseous product wherein, naphtha fraction, the rocket engine fuel cut, diesel oil distillate is respectively through pipeline 9,10,11,12 caterpillars, the tail oil cut then loops back hydrocracking reactor 19 through pipeline 13, under the effect of hydroisomerizing cracking catalyst hydrocracking reaction takes place, highly selective is converted into the purpose product.
The invention has the advantages that:
1, the integrated form technical process can be finished the hydrogenation process for upgrading process of Fischer-Tropsch synthesis oil diesel oil distillate and wax oil cut simultaneously, can reduce investment and process cost effectively.
2, the fractionated again technical process of the full cut of Fischer-Tropsch synthesis oil elder generation's hydrofining can avoid oil property in the Fischer-Tropsch synthesis oil fractionation process of high olefin content to change influence to following process.
3, have production handiness preferably, by the adjustment of operating parameters, as control hydrofining reaction and the depth of conversion of hydrocracking reaction and the cut point of separation column etc., the product that can obtain different demands distributes.
4, the technical process that proposes of the present invention helps improving the yield of intermediate oil, can reduce the secondary cracking of light constituent; Help reducing the volume and the loaded catalyst of isomery hydrocracking reactor; The hydrogenation pre-treatment has been passed through in isomery hydrocracking charging simultaneously, helps to prolong the running period of catalyzer.
5, by the reasonable arrangement of technical process, avoid unifining process to generate water and entered into the isocracking reactor, can improve the utilization ratio and the life cycle of catalyzer.
The following examples will give further instruction to present method, but therefore not limit present method.
With the full cut of Fischer-Tropsch synthesis oil is raw material, and its character sees Table 1.The trade names of hydrogenation protecting agent, Hydrobon catalyst, hydroisomerizing cracking catalyst are respectively RGF-1, RTF-1, RCF-1, and the volume ratio of RGF-1/RTF-1 is 15: 100.Test is carried out according to technical process provided by the present invention on medium-sized fixed bed hydrogenation device.
Embodiment
Test is listed in table 2 with catalyzer and operational condition, and product naphtha fraction character is listed in table 3, and product diesel oil distillate character is listed in table 4.
Data adopt the method that provides of the present invention 300 ℃ of hydrogen dividing potential drop 6.4MPa, hydrofining reaction temperature as can be seen from table, and hydroisomerizing cracking reaction temperature is 363 ℃, cumulative volume air speed 2.0h
-1, the synthetic full distillate oil of processing Fischer-Tropsch can be converted into petroleum naphtha and diesel product entirely with the wax oil cut under the condition of hydrogen to oil volume ratio 800v/v.Diesel product yield is higher, is 83.6 heavy %, and its cetane value is 80, can concoct with the low cetane number diesel cut; Naphtha fraction mainly is made of alkane, is preparing ethylene by steam cracking raw material preferably.
Table 1, the synthetic full distillate oil main character of Fischer-Tropsch
| Project | Data |
| Density (20 ℃), g/cm 3 | 0.7990 |
| Boiling range (ASTM D-1160), ℃ | |
| IBP/10％ | 68/205 |
| 30％/50％ | 331/369 |
| 90％/95％ | 553/637 |
| Oxygen level, heavy % | 0.75 |
Table 2, operational condition
| Project | Data |
| Hydrofining reactor: | |
| Catalyzer | RGF-1/RTF-1 |
| The hydrogen dividing potential drop, MPa | 6.4 |
| Temperature of reaction, ℃ | 300 |
| Hydrocracking reactor: | |
| Catalyzer | RCF-1 |
| The hydrogen dividing potential drop, MPa | 6.4 |
| Temperature of reaction, ℃ | 353 |
Table 3, naphtha fraction product property
| Project | |
| The boiling range scope | ＜150℃ |
| Yield, heavy % | 16.3 |
| Density (20 ℃), g/cm 3 | 0.705 |
| Form heavy % | |
| Normal paraffin | 46.50 |
| Isoparaffin | 49.96 |
Table 4, diesel oil distillate product property
| Project | |
| The boiling range scope | 150-340℃ |
| Yield, heavy % | 83.6 |
| Density (20 ℃), g/cm 3 | 0.760 |
| Condensation point, ℃ | -13 |
| Cetane value | 80 |
Claims (5)
1, a kind of integrated Fischer-Tropsch synthetic oil hydrogenation purification, it is characterized in that the full cut of Fischer-Tropsch synthesis oil, hydrogen contact with Hydrobon catalyst, hydrofining reaction logistics and hydrocracking reaction logistics mix through separating and obtain intermediate oil product and petroleum naphtha and tail oil, are circulated to the isocracking reactor after tail oil and the hydrogen mixing and contact with the hydroisomerizing cracking catalyst.
2, according to the method for claim 1, it is characterized in that hydrogenation reaction is to carry out under hydrogen dividing potential drop 2.0-16.0MPa, 250-430 ℃ of hydrofining reaction temperature, hydroisomerizing cracking reaction temperature is 300-450 ℃, cumulative volume air speed 0.1-4.0h
-1, hydrogen to oil volume ratio 100-1500v/v.
3, according to the method for claim 1, it is characterized in that described Hydrobon catalyst is a kind of metal load type catalyst, carrier is unformed aluminum oxide, and metal component is that VIB is or/and VIII family base metal, wherein the group vib metal is Mo or/and W, and VIII family metal is that Co is or/and Ni.
4, according to the method for claim 1 or 3; it is characterized in that the hydrogenation protecting agent is seated in the Hydrobon catalyst top; described protective material is to load on VIB on unformed aluminum oxide or the silica-alumina supports or/and VIII family non-precious metal catalyst, and the volume ratio of protective material and Hydrobon catalyst is 0-30: 100.
5, according to the method for claim 1, it is characterized in that noble metal catalyst or non-precious metal catalyst that described hydroisomerizing hydrocracking catalyst is the amorphous aluminum silicide load, the metal component of non-precious metal catalyst is that VIB is or/and VIII family base metal, wherein the group vib metal is Mo or/and W, and VIII family metal is that Co is or/and Ni; The metal component of noble metal catalyst is that Pt is or/and Pd.
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| CN101230291B (en) * | 2007-01-23 | 2012-02-29 | 中国石油化工股份有限公司 | Low consumption energy method for processing fischer-tropsch synthesis |
| CN102911722A (en) * | 2011-08-01 | 2013-02-06 | 中国石油化工股份有限公司 | Hydrogenation quality-improving method for Fischer-Tropsch synthetic oil |
| CN102911729A (en) * | 2011-08-01 | 2013-02-06 | 中国石油化工股份有限公司 | Method for producing diesel oil from Fischer-Tropsch synthetic oil |
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| US5878348A (en) * | 1996-05-30 | 1999-03-02 | Telefonaktiebolaget Lm Ericsson (Publ) | System and method for implementing multiple home location registers for a single mobile station in a cellular telecommunications network |
| US5766274A (en) * | 1997-02-07 | 1998-06-16 | Exxon Research And Engineering Company | Synthetic jet fuel and process for its production |
| FR2826972B1 (en) * | 2001-07-06 | 2007-03-23 | Inst Francais Du Petrole | PROCESS FOR THE PRODUCTION OF MEDIUM DISTILLATES BY HYDROISOMERIZATION AND HYDROCRACKING OF A HEAVY FRACTION RESULTING FROM AN EFFLUENT PRODUCED BY THE FISCHER-TROPSCH PROCESS |
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