CN1212376C - Light hydrocarbon non-hydrogenation modified catalyst, preparing process and application thereof - Google Patents
Light hydrocarbon non-hydrogenation modified catalyst, preparing process and application thereof Download PDFInfo
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- CN1212376C CN1212376C CN 03105391 CN03105391A CN1212376C CN 1212376 C CN1212376 C CN 1212376C CN 03105391 CN03105391 CN 03105391 CN 03105391 A CN03105391 A CN 03105391A CN 1212376 C CN1212376 C CN 1212376C
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Abstract
The present invention relates to a non-hydrogenation modifying catalyst of C3 to C11 light hydrocarbon mixture, which comprises 0.1 wt% to 5.0 wt% of mixed rare earth oxide or antimony oxide and 95.0 wt% to 99.1 wt% carrier, wherein the carrier is prepared from 50 wt% to 80 wt% of HZSM-5 zeolite and 20 wt% to 50 wt% of gamma-aluminum oxide. The catalyst is suitable for modifying gasoline with a low octane value to enhance gasoline octane value and lower olefin content.
Description
Technical field
The present invention is a kind of lighter hydrocarbons non-hydrogen modifying catalyst and preparation method and application, specifically, be a kind of catalyzer and preparation method who is used for low octane rating straight-run spirit or oil field light hydrocarbon upgrading, and with the method for modifying of described catalyzer to straight-run spirit or oil field light hydrocarbon.
Background technology
Along with the raising day by day of environmental requirement, olefin(e) centent will be lower than 35% in the gasoline composition content new standard regulation gasoline of country's promulgation recently.And China's gasoline is at present mainly based on catalytically cracked gasoline, and olefin(e) centent is higher than 35% far away, and the gasoline fraction that the catalytic cracking process that especially heavy oil and slag-mixing amount are very high is produced is depended merely on the improvement catalytic cracking technology, and olefin(e) centent still is difficult to reach set quota.For some middle-size and small-size refineries that lacks catalytic reforming and hydrogenation unit, take to mix the method for converting a part of straight-run spirit, can reduce the olefin(e) centent of gasoline product.But the octane value of straight-run spirit is very low, mixes the reduction significantly that will inevitably cause gasoline octane rating in the catalytically cracked gasoline.Thereby need straight-run spirit is carried out upgrading, do not produce too much alkene simultaneously again at its octane value of raising.
CN1080313A discloses a kind of catalytic modification of poor quality gasoline-aromatization method, and its catalyzer is the rare earth modified HZSM-5 zeolite of Zn-Al or Zn-Al-, and is binding agent with aluminum oxide or silicon oxide.This technology adopts two-part reaction unit, and first step reactor makes raw material and catalyzer contact reacts under non-hydrogen, 300～550 ℃, the condition of 0.05～1.2MPa, weight hourly space velocity 0.2～10, and resultant of reaction is through gas-liquid separation, C
5Above liquid discharge device aftercut, again the gasoline fraction that obtains is sent into second stage reactor, carry out aromatization under 0.05～1.5MPa, volume space velocity 20～2000,480～650 ℃ of conditions of bed temperature, resultant of reaction obtains aromatic hydrocarbons mixture and the gas that is rich in hydrogen through gas-liquid separation.
The articles that are entitled as " isomerization technique that improves octane number of direct distillation gasoline " of " oil refining designs " the 31st volume the 2nd phase P23～25 reports adopt 90 of straight-run spirit isomerization catalyst production
#Gasoline though octane value is higher, wherein contains more alkene and aromatic hydrocarbons, and its content is respectively 13.78% and 14.95%.
Summary of the invention
The purpose of this invention is to provide a kind of low-octane light hydrocarbons modifying catalyst and preparation method, this catalyzer can be converted into light hydrocarbons liquefied gas and stop bracket gasoline blend component.
Another object of the present invention provides a kind of low-octane light hydrocarbons method for modifying.
The zeolite that contains in the catalyzer of the present invention has proper acidic, can be with the straight-chain paraffin cracking Generation Liquid gasification and the isomeric hydrocarbon of low-octane straight-run spirit or oil field light hydrocarbon, and make the dehydrogenation of part naphthenic hydrocarbon be converted into aromatic hydrocarbons, thus improve the octane value of oil product.The oil product olefin(e) centent that obtains with catalyzer of the present invention and technology upgrading is extremely low, is used as the gasoline blend component and mixes and to convert catalytically cracked gasoline, can reduce the olefin(e) centent of catalytically cracked gasoline greatly, and gasoline octane rating is reduced significantly.In addition, the present invention carries out suitable high-temperature water vapor to catalyzer and handles, and makes catalyzer both have good selective splitting activity, has satisfactory stability and regenerability again.
Use straight-run spirit or the oil field light hydrocarbon that method for modifying of the present invention can low octane rating (RON=45～54) to be raw material, 0.2～0.7MPa, 300～460 ℃, raw material weight air speed 0.4～1.5 o'clock
-1Condition under, the gasoline blend component of the high-octane rating (RON＞84) of production 60～70 quality % and the high-quality liquefied gas of 28～37 quality %, dry gas yied is lower than 2 quality %, and the olefin(e) centent of the oil ingredient that steams is lower than 5 quality %, and benzene content is not more than 1.5 quality %.The catalyzer one way can reach 1～3 month work-ing life.
Description of drawings
Fig. 1 is a modifying process schema provided by the invention.
Fig. 2 is a modifying catalyst life assessment experimental result of the present invention.
Embodiment
C provided by the invention
3～C
11The non-hydrogen modifying catalyst of mixture of light hydrocarbons, comprise the carrier of the mixed rare-earth oxide of 0.1～5.0 quality % or weisspiessglanz, 95.0～99.1 quality %, described carrier is made up of the HZSM-5 zeolite of 50～80 quality % and the gama-alumina of 20～50 quality %.
Mixed rare-earth oxide in the catalyzer contains the lanthanum trioxide of 20～40 quality %, the cerium oxide of 40～60 quality %, the Praseodymium trioxide of 10～18 quality %, the Neodymium trioxide of 2～10 quality %.Preferred 0.1～3.0 quality % of the content of mixed rare-earth oxide or weisspiessglanz.
The silica alumina ratio of described HZSM-5 zeolite is 30～100, preferred 30～80.HZSM-5 can be made through ion-exchange by NaZSM-5, also can be by NH
4ZSM-5 makes through roasting.
Described lighter hydrocarbons are straight-run spirit or oil field light hydrocarbon, wherein contain the straight-chain paraffin of 50.0～80.0 quality %, the naphthenic hydrocarbon of 16.0～45.0 quality % and the aromatic hydrocarbons of 0.1～7.0 quality %.
Preparation of catalysts method provided by the invention can have two kinds, a kind of is to prepare carrier earlier, by dipping active ingredient is introduced carrier again, carry out steam-treated then and make catalyzer, another kind method is that the active ingredient oxide compound is added wherein when the preparing carriers, after moulding, the roasting, carry out steam-treated again and make catalyzer.
First method provided by the invention comprises:
(1) HZSM-5 and α-water aluminum oxide powder are pressed 50～80: 50～20 butt weight ratio mixing moulding, dry, roasting make carrier,
(2) the soluble salt solution impregnation (1) with chlorination mishmetal or antimony goes on foot the carrier that makes, dry roasting,
(3) (2) one-step baking rear catalyst is warming up to 500～600 ℃ in airflow, used the pure water steam treatment again 1～12 hour, the weight ratio of total water amount and catalyzer is 1～10 during processing.
The dipping temperature in described (2) step is 20～70 ℃, and the consumption of steeping fluid is 0.5～2.0 milliliter in every gram carrier during dipping, preferred 0.8～1.3.The soluble salt of described antimony is selected from antimony chloride or nitric acid antimony, contains elements such as lanthanum, cerium, praseodymium, neodymium in the described chlorination mishmetal, and its content is counted with oxide compound: lanthanum 20～40 heavy %, cerium 40～60 heavy %, praseodymium 10～18 heavy %, neodymium 2～10 heavy %.
In the aforesaid method, the order in (2), (3) step can be put upside down, and is about to the carrier that (1) step makes and carries out steam-treated by the method in (3) step earlier, and then introduce mishmetal or antimony by the method in (2) step.The content of mishmetal or antimony should reach the content requirement in the catalyzer that finally makes in described (2) step steeping fluid.
The another kind of preparation method of catalyzer of the present invention is by butt weight ratio mixing moulding with HZSM-5, α-one water aluminum oxide and mixed rare earth oxide or weisspiessglanz, each component concentration should reach the desired content of catalyzer during mixing, after the moulding after material drying, the roasting, in airflow, be warming up to 500～600 ℃, used the pure water steam treatment again 1～12 hour, the weight ratio of total water amount and catalyzer is 1～10 during processing.
The purpose of in the described method catalyzer being carried out steam-treated is to regulate its acidity, preferred 520～580 ℃ of its treatment temp, and in preferred 3～7 hours of treatment time, the weight ratio of total water amount and catalyzer preferred 1～2 during processing.The condition of steam-treated should suitably be adjusted according to the silica alumina ratio of HZSM-5 zeolite, the height of acid cracked activity, is in the state of coordinating most with acid function and the dehydrogenation functionality that guarantees catalyzer.The standard of adjusting the steam-treated condition is to make raw materials used HZSM-5 (measuring method of α value is write " petrochemical complex analytical procedure (RIPP experimental technique) " with reference to Yang Cuiding etc. between 20～200 through the α value after the steam-treated, Science Press publishes, P255 " constant temperature method is measured the α value of an acidic catalyst ").
In the above-mentioned catalyst preparation process, described drying temperature is 60～120 ℃, and the time is 2～10 hours, and maturing temperature is 400～650 ℃, and preferred 450～550 ℃, the time is 2～8 hours, preferred 2～4 hours.
The shape of described catalyzer can be bar shaped, sheet shape, sphere or particulate state, preferred bar shaped.The catalyzer of different shape all can adopt conventional method preparation.As prepare the bar shaped carrier and can will raw material mix nitric acid or the acetic acid that the back adds suitable quantity of water and 1～3 heavy % and mediate extruded moulding, dry then, roasting.
C provided by the invention
3～C
11The non-hydrogen method for modifying of mixture of light hydrocarbons was included in 0.2～0.7MPa, 300～460 ℃, raw material weight air speed 0.4～1.5 o'clock
-1Condition under make described mixture of light hydrocarbons and catalyzer contact reacts of the present invention, described light hydrocarbon feedstocks need not to make with extra care.Upgrading can adopt the reaction unit of fixed bed half regenerative, uses single or multiple reactors, and technical process and product separation reclaim all comparatively simple.
By the technical process of non-hydrogen upgrading of the present invention shown in Figure 1 as can be known, earlier straight-run spirit or oil field light hydrocarbon are sent into interchanger 5 with pump 1, after the reaction product heat exchange of coming out with reactor 3, enter process furnace 2 internal heating again to temperature of reaction, enter reactor 3 and catalyzer contact reacts wherein then from the top, selective splitting takes place in low-octane reaction raw materials under the effect of catalyzer, isomerization, oligomerisation, series of chemical such as cyclisation and aromizing, the octane value of gasoline is increased substantially, while by-product part high-quality liquefied gas, the reaction after product is discharged from reactor 3 bottoms, through interchanger 5 and raw material heat exchange after condenser 6 condensations, enter knockout drum 4 again and carry out gas-liquid separation, the tank deck rich gas goes to stabilizer tower 8 middle parts, jar end liquid enters stabilizer tower 8 bottoms, and liquefied gas separates in stabilizer tower with high octane gasoline component, and a small amount of dry gas is discharged from the stabilizer tower top, liquefied gas is discharged from stabilizer tower top, and stop bracket gasoline is in harmonious proportion component and discharges at the bottom of by stabilizer tower.
Can regenerate behind the catalyst deactivation of the present invention, renovation process is to do resurgent gases with oxygen containing stack gas or nitrogen to burn carbon, and oxygen level is 0.3～2.1%, and resurgent gases volume air speed is 500～1500h
-1, regeneration temperature is 350～450 ℃, regeneration pressure is normal pressure～0.3MPa.
Further specify the present invention below by example, but the present invention is not limited to this.
Example 1
Prepare catalyzer of the present invention.
(1) preparation carrier: get silica alumina ratio and be 56 HZSM-5 zeolite powder 130 grams (the prosperous catalyst plant production of Shanghai China); α-one water aluminum oxide powder (German Condea company produce) 70 grams; mix; add the solution that 2 milliliters of 1: 1 nitric acid and 50 ml waters are made into; mediate agglomeratingly, in banded extruder, be squeezed into 2 millimeters of diameters, long 3～5 millimeters bar; 110 ℃ of dryings 12 hours, 570 ℃ of roastings 4 hours.
(2) introduce active ingredient: get above-mentioned carrier 100 grams, (Baotou rare earth industrial in the Inner Mongol produces to contain 1.35 gram chlorination mishmetals with 100 milliliters, wherein lanthanum trioxide 31%, cerium oxide 51%, Praseodymium trioxide 14%, Neodymium trioxide 4%, x-ray fluorescence method analysis) the aqueous solution 60 ℃ of dippings 2 hours, 110 ℃ of dryings 10 hours, 550 ℃ of roastings 4 hours.
(3) steam-treated: the catalyzer that makes of (2) step is packed in the tubular reactor, in airflow, be warming up to 570 ℃ under the normal pressure, under this temperature, change water flowing steam treatment 7 hours then, feed dry air again and purge cooling.Total inflow is 400 grams in the steam-treated process.
Mixed rare earth oxide content is 0.45 quality % (x-ray fluorescence method analysis, down together) in the above-mentioned catalyst A that makes.
Example 2
Method by example 1 prepares catalyst B, and different is that the carrier that (1) step makes is carried out steam-treated earlier, and then introduces mishmetal with the method in (2) step, and mixed rare earth oxide content is 0.45 quality % in the catalyst B that obtains.
Example 3
Method by example 1 prepares catalyzer C, in different is (2) step in the steeping fluid content of chlorination mishmetal be 9.0 grams, (3) step treatment time of water is 2 hours.Mixed rare earth oxide content is 3.0 quality % among the catalyzer C that makes.
Example 4
Get silica alumina ratio and be 56 HZSM-5 zeolite powder 65 grams (the prosperous catalyst plant of Shanghai China); α-one water aluminum oxide powder (German Condea company produce) 35 grams; weisspiessglanz 2 grams; mix, add the solution that 2.4 milliliters of 1: 1 nitric acid and 50 ml waters are made into, mediate agglomerating; in banded extruder, be squeezed into 2 millimeters of diameters; long 3～5 millimeters bar, 110 ℃ of dryings 12 hours, 580 ℃ of roastings 4 hours.Carry out steam-treated by the method in 1 (3) step of example again, the content of weisspiessglanz is 2.2 quality % of butt among the catalyzer D that makes.
Example 5
The experiment of straight-run spirit upgrading.
In 20 milliliters of fixed-bed reactor, load 14 gram catalyst B and D respectively, respectively with 1
#Straight-run spirit and oil field light hydrocarbon (2
#Oil) be raw material, when 420 ℃ of bed temperatures, 0.2MPa, raw material weight hourly space velocity 2.0
-1Condition under carry out non-hydrogen upgrading experiment respectively, reaction result sees Table 2, raw materials used oil nature sees Table 1.
By table 2 result as can be known, under same reaction conditions, the oil field light hydrocarbon (2 that the raw material fraction is low weight
#Oil), dry gas and liquefied gas yield are all than higher, but dry gas yied is still less than 2.0 quality %.
Example 6
Press the method for example 5, with in the table 13
#Straight-run spirit is raw material, and 370 ℃ of bed temperatures, 0.4MPa is during raw material weight hourly space velocity 0.5
-1Conditions of non-hydrogen under, respectively catalyst A, C are estimated, result and product property see Table 3.
As shown in Table 3, dry gas yied is less than 0.6 quality % in the product behind the upgrading, and liquid product yield reaches more than 67%, and the research octane number (RON) of liquid product is greater than 84, olefin(e) centent illustrates that less than 2.1 quality % the gained liquid product is a kind of olefin gasolines mediation component that well falls.
Example 7
Load 14 gram catalyst A respectively at 20 milliliters of fixed-bed reactor, with in the table 11
#Straight-run spirit is raw material, and 320～450 ℃ of bed temperatures, 0.3MPa is during raw material weight hourly space velocity 0.5
-1Conditions of non-hydrogen under catalyzer is carried out the upgrading life experiment, reaction result is seen Fig. 2.
As shown in Figure 2, catalyst A of the present invention is after using 1100 hours, and each product yield does not still have obvious decline, illustrates that catalyzer of the present invention has good activity stability.
Table 1
Raw material numbering 1
#2
#3
#
Boiling range, ℃
Initial boiling point 36 24 70
10％ 62 33 92
30％ 90 42 105
50％ 108 51 118
70％ 123 64 133
90％ 142 86 150
Final boiling point 158 119 168
Group composition, quality %
Alkane 58.60 79.95 52.26
Naphthenic hydrocarbon 36.50 17.37 41.11
Aromatic hydrocarbons 4.90 2.68 6.33
Basic nitrogen, ppm 1.4
As，ppb ＜2 ＜2
S，ppm 157 140
d
25 ℃Density, g/cm
30.713 0.7341
Table 2
| The raw material numbering | 2 # | 1 # | ||
| The catalyzer numbering | B | D | B | D |
| Dry gas yied, quality % liquefied gas yield, quality % C5 +Liquid is received, quality % aromatic hydrocarbons, and quality % adds up to, quality % | 1.82 45.21 50.97 10.42 98.0 | 1.86 49.63 47.24 11.96 98.73 | 1.11 30.94 65.64 13.59 97.65 | 1.00 37.22 58.79 15.01 97.01 |
Table 3
| The raw material numbering | 3 # | |
| The catalyzer numbering | A | C |
| Dry gas yied, quality % liquefied gas yield, quality % C5 +Liquid is received, and quality % adds up to, quality % aromatic hydrocarbons/C5 +, quality % | 0.53 31.65 67.73 99.91 20.43 | 0.48 30.08 69.26 99.82 20.16 |
| Liquid product | ||
| Group composition, volume % stable hydrocarbon alkene aromatic hydrocarbons | 79.97 2.04 16.81 | 76.0 0.8 23.2 |
| The octane research method motor method | 85.0 76.4 | 89.1 79.0 |
| Boiling range, ℃ initial boiling point | 40 202 | 38 205 |
Claims (13)
1, a kind of C
3～C
11The non-hydrogen modifying catalyst of mixture of light hydrocarbons, carrier by the mixed rare-earth oxide of 0.1～5.0 quality % or weisspiessglanz, 95.0～99.1 quality % is formed, and wherein said carrier is made up of the HZSM-5 zeolite of 50～80 quality % and the gama-alumina of 20～50 quality %.
2,, it is characterized in that described mixed rare-earth oxide contains the Praseodymium trioxide of the cerium oxide of the lanthanum trioxide of 20～40 quality %, 40～60 quality %, 10～18 quality %, the Neodymium trioxide of 2～10 quality % according to the described catalyzer of claim 1.
3,, it is characterized in that the content of mixed rare-earth oxide in the catalyzer or weisspiessglanz is 0.1～3.0 quality % according to the described catalyzer of claim 1.
4, according to the described catalyzer of claim 1, the silica alumina ratio that it is characterized in that described HZSM-5 zeolite is 30～100.
5, according to the described catalyzer of claim 1, it is characterized in that described lighter hydrocarbons are straight-run spirit or oil field light hydrocarbon, wherein contain the straight-chain paraffin of 50.0～80.0 quality %, the naphthenic hydrocarbon of 16.0～45.0 quality % and the aromatic hydrocarbons of 0.1～7.0 quality %.
6, the described Preparation of catalysts method of a kind of claim 1 comprises:
(1) HZSM-5 and α-water aluminum oxide powder are pressed 50～80: 50～20 butt weight ratio mixing moulding, dry, roasting make carrier,
(2) the soluble salt solution impregnation (1) with chlorination mishmetal or antimony goes on foot the carrier that makes, dry roasting,
(3) (2) one-step baking rear catalyst is warming up to 500～600 ℃ in airflow, used the pure water steam treatment again 1～12 hour, the weight ratio of total water amount and catalyzer is 1～10 during processing.
7, in accordance with the method for claim 6, it is characterized in that described maturing temperature is 400～600 ℃.
8, in accordance with the method for claim 6, it is characterized in that the dipping temperature in (2) step is 20～70 ℃, the consumption of steeping fluid is 0.5～2.0 milliliter in every gram carrier during dipping.
9, in accordance with the method for claim 6, the soluble salt that it is characterized in that described antimony of (2) step is selected from antimony chloride or nitric acid antimony, and each constituent content in oxide compound in the chlorination mishmetal is: lanthanum 20～40 heavy %, cerium 40～60 heavy %, praseodymium 10～18 heavy %, neodymium 2～10 heavy %.
10, in accordance with the method for claim 6, it is characterized in that (1) goes on foot the carrier that makes and carries out steam-treated by the method in (3) step earlier, and then press the method introducing mishmetal or the antimony in (2) step.
11, the described Preparation of catalysts method of a kind of claim 1, comprise HZSM-5, α-one water aluminum oxide and mixed rare earth oxide or weisspiessglanz by butt weight ratio mixing moulding, in airflow, be warming up to 500～600 ℃ after drying, the roasting, used the pure water steam treatment again 1～12 hour, the weight ratio of total water amount and catalyzer is 1～10 during processing.
12, a kind of C
3～C
11The non-hydrogen method for modifying of mixture of light hydrocarbons was included in 0.2～0.7MPa, 300～460 ℃, raw material weight air speed 0.4～1.5 o'clock
-1Condition under make described mixture of light hydrocarbons and the described catalyzer contact reacts of claim 1.
13, in accordance with the method for claim 12, it is characterized in that described mixture of light hydrocarbons is straight-run spirit or oil field light hydrocarbon, wherein contain the straight-chain paraffin of 50.0～80.0 quality %, the naphthenic hydrocarbon of 16.0～45.0 quality % and the aromatic hydrocarbons of 0.1～7.0 quality %.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100383222C (en) * | 2005-07-28 | 2008-04-23 | 中国石油化工股份有限公司 | Catalytic reforming method using light hydrocarbon as raw material |
| CN101172252B (en) * | 2006-11-01 | 2010-05-12 | 中国石油化工股份有限公司 | Reforming catalyst and application in high selectivity production of para-xylene of the same |
| CN101397510B (en) * | 2007-09-28 | 2012-07-18 | 中国石油化工股份有限公司 | Inferior gasoline upgrading method |
| CN101333461B (en) * | 2008-03-25 | 2012-02-29 | 北京惠尔三吉绿色化学科技有限公司 | Method for producing cleaning fuel oil form petroleum cracking dry gas and C4 component |
| CN101724432B (en) * | 2008-10-31 | 2012-09-12 | 中国石油化工股份有限公司 | Method for producing high-octane gasoline by light hydrocarbon non-hydrogenation modification |
| CN102950017B (en) * | 2011-08-26 | 2016-03-02 | 中国石油化工股份有限公司 | Oil refinery dry gas is utilized to produce the Catalysts and its preparation method of gasoline |
| CN102794195B (en) * | 2012-08-28 | 2014-08-27 | 丁泳 | Catalyst suitable for enhancing gasoline octane number of fuel and lowering olefin content and application thereof |
| CN105772070B (en) * | 2016-02-23 | 2019-07-16 | 新疆恒晟能源科技股份有限公司 | A kind of catalyst and preparation method thereof for the modification of gasoline non-hydrogen |
| CN110947417B (en) * | 2018-09-27 | 2022-11-15 | 中国石油化工股份有限公司 | Catalyst for producing propane and gasoline from alkane, preparation method and application |
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