CN1147536A - Multiple-metal reforming catalyst - Google Patents

Multiple-metal reforming catalyst Download PDF

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CN1147536A
CN1147536A CN 95116457 CN95116457A CN1147536A CN 1147536 A CN1147536 A CN 1147536A CN 95116457 CN95116457 CN 95116457 CN 95116457 A CN95116457 A CN 95116457A CN 1147536 A CN1147536 A CN 1147536A
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catalyzer
heavy
catalyst
described catalyzer
rhenium
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CN1039818C (en
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孙作霖
戚杰
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Sinopec Research Institute of Petroleum Processing
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Abstract

The reforming catalyst with noble material components consists of in weight percentage: Pt 0.10-1.00, Re 0.10-3.00, Ti 0.01-0.15, Al 0.01-0.15, Cl 0.50-3.00, and gamma-Al2O3 carrier the rest. With high activity, selectivity and stability, the catalyst of the present invention is used in reforming process of directly-fractionated naphtha and gasoline produced through coking and cracking process.

Description

A kind of multimetal reforming catalyst
The invention belongs to catalyst for reforming naphtha, specifically contain the multimetal reforming catalyst of platinum rhenium precious metal constituent element.
Catalytic reforming is one of important production technique of refining of petroleum, and stop bracket gasoline component and broad-spectrum aromatic hydrocarbons and cheap hydrogen can be provided.Because many developed countries are limited and are used white gasoline to the objectionable impurities of motor vehicle exhaust, the demand of Gaoxin value blending component is constantly increased, therefore promoted the development of reforming process, wherein the progress with catalyzer is more remarkable.
Modern reforming catalyst is a dual-function catalyst.A kind of is hydrogenation-dehydrogenation functionality, is provided by the metal constituent element; Another kind is the isomerization acid function, is provided by carrier and non-metallic element, and carrier commonly used has γ-Al 2O 3And η-Al 2O 3
From nineteen sixty-eight United States Patent (USP) 3,415,373 have disclosed adding rhenium constituent element in platinum-reforming catalyst, significantly improve after the stability of catalyzer, platinum rhenium bimetallic catalyst is widely used, but it still has some deficits, still remain to be improved as selectivity, for further improving the performance of catalyzer, people introduce the reactivity worth of the third metal in order to regulating catalyst again in bimetallic catalyst, usually claim that this third metal is metal promoters or " modulation agent ", as USP4,235,705 introduce bismuth metal in platinum-rhenium catalyst, make in catalyzer, to form bismuth oxide and Bismuth Aluminate, thereby improve activity of such catalysts, stability and selectivity, its objective is is not influencing C 5 +Improve C under the situation of average yield or catalyst life 5 +The octane value of product (organon reaches 100), and the rich H that produces 2
For the alumina supporter that the isomerization acid function is provided, select for use its performance of different preparation methods also different, and then have influence on the performance of catalyzer.As USP4,178,268 adopt Ziegler to synthesize by-product SB aluminum oxide is the preparing carriers reforming catalyst, has improved activity of such catalysts, selectivity and stability; The HP aluminum oxide that CN1032951A adopts the hydrolysis of low-carbon alkyl aluminium to make is done carrier, and loaded metal platinum, rhenium, titanium also make the reactivity worth of catalyzer increase.
The object of the present invention is to provide a kind of platinum rhenium multimetal reforming catalyst of introducing promotor, this catalyzer has high activity and selectivity and good stability.
Catalyzer of the present invention has following composition (is benchmark with the butt aluminum oxide, heavy %): Pt0.10～1.00, preferably 0.10～0.50; Re0.10～3.00, preferably 0.10～2.00; Ti0.01～0.15, preferably 0.08～0.15; Al0.01～0.15, preferably 0.01～0.08; Cl0.50～3.00, preferably 0.5～1.5, surplus be γ-Al 2O 3Carrier.The rhenium platinum weight ratio of this catalyzer is 0.50～4.0, preferably 1.0～3.0.
Described Al form with unformed aluminum oxide in catalyzer exists.
Described γ-Al 2O 3High-purity γ-Al of making of alkyl aluminum hydrolysis preferably 2O 3
Catalyzer of the present invention can make with the method for soaking altogether of routine, and its preparation process is: precursor, hydrochloric acid and decationized Y sieve water mixed liquid with each metal constituent element of predetermined amount at room temperature flood γ-Al 2O 3Carrier, liquid-solid volume ratio is 1.2～2.2, preferably 1.5～1.8 during dipping; Dipping time is 6～24 hours, filter then, difference is dry 6～12 hours, 12～24 hours under 60～80 ℃, 110～130 ℃, 450～550 ℃, gas agent volume ratio are activation in 700～1200 o'clock 2～12 hours in the dry air, afterwards in 400～500 ℃, gas agent volume ratio be 400～1000 o'clock with hydrogen reducing 2～12 hours.
The precursor of said each metal constituent element is preferably Platinic chloride to the platinum constituent element, and the rhenium constituent element is preferably perrhenic acid and rhenium carbonyl, and the titanium constituent element is preferably titanous chloride, and the aluminium constituent element is aluminum chloride, aluminum nitrate, is preferably aluminum chloride.
Catalyzer of the present invention also can adopt the step impregnation method preparation, but must soak another kind of component again after super-dry, activation after a kind of component on every dipping.
Ti constituent element in the catalyzer of the present invention also can be introduced with coprecipitation method in the preparing carriers process.
The another kind of constituent element of catalyzer of the present invention is the halogen that comprises fluorine, chlorine, best with chlorine, and chlorine can be introduced in catalyst preparation process.Also can in the catalyzer use, introduce, best mode be the form of or Organohalogen compounds inorganic with hydrochloric acid or other when dipping and the metal constituent element together introduce.
Catalyzer of the present invention can be sphere, particulate state, sheet shape or bar shaped (comprising abnormity such as cylindrical, trilobal, quatrefoil) with common method moulding, the gained respective shapes such as ball, spin, compressing tablet, extrusion of dripping, and is the most frequently used with sphere or bar shaped.
Catalyzer of the present invention is the same with other platinum-rhenium reforming catalyst must to pass through prevulcanized before use.Prevulcanized can be by injecting H in the hydrogen stream 2The mode of S or other organic or inorganic sulfide is carried out, and the sulphur content on the catalyzer is 0.01～2.00 heavy %, is preferably 0.04～0.15 heavy %.
Catalyzer of the present invention can be used for boiling range and is 40～230 ℃ and (presses GB 255 methods analysts, as follows) virgin naphtha or comprise that the boiling range of explained hereafter such as coking in the refining of petroleum, cracking is the reformation of 40～230 ℃ petroleum naphtha, be specially adapted to the reformation of virgin naphtha.
Catalyzer of the present invention has been because dipping the time has been introduced aluminium salt in platinum-rhenium reforming catalyst, thereby improved activity of such catalysts and arenes selectivity.As experimentizing on the 100ml device, catalyzer of the present invention is than the transformation efficiency high 1.5 heavy % of industrial platinum-rhenium catalyst (CB-6), and aromatics yield high 0.6 weighs %, and catalyzer of the present invention has satisfactory stability.
Further specify the present invention below by example.
The stage first alive of evaluation experimental indication is the catalytic performance of live catalyst under normal operating condition in the example, accelerating the aging step is the catalytic performance of catalyzer under the high severity operational condition, it is the common method of laboratory evaluation catalyst stability, the recovery stage be catalyzer through accelerate aging after, return to the catalytic performance under the normal operating condition.
Example 1
This case introduction prepares the method for catalyzer of the present invention.
At room temperature with 100 gram SB balls (German Condea company, contain the heavy % of Ti0.1) pour Platinic chloride (the Chang Ling catalyst plant of predetermined amounts preparation into, analytical pure), perrhenic acid (Wuhan specialty oil products factory, analytical pure), aluminum chloride (Red Star chemical plant, Beijing, analytical pure) and hydrochloric acid (Red Star chemical plant, Beijing, analytical pure) in the steeping fluid that is made into, contains the heavy % of heavy %, Cl1.60 of heavy %, Al0.01 of Pt0.22 heavy %, Re0.44 in this steeping fluid (all with butt Al 2O 3Be benchmark).Liquid-solid volume ratio is 1.20, flood 24 hours after-filtration, moist catalysis is 60 ℃ and 120 ℃ respectively dry 6 and 12 hours down, then 500 ℃, the activation in 700: 1 of gas agent volume ratio 4 hours in dry air, 500: 1 hydrogen reducings of 500 ℃ of gas agent volume ratios 4 hours promptly get catalyst A of the present invention-1.Carry out prevulcanized afterwards,, in hydrogen stream, inject H in 500 ℃ 2The S fluidisation, H 2Till S adds to beds and penetrates.(following each catalyzer all passes through prevulcanized)
A-2, the same basically A-1 of A-3 Preparation of catalysts method, just Al content difference.The introducing amount of A-2 catalyst A l is 0.03 heavy % during dipping, and the introducing amount of A-3 catalyst A l is 0.05 heavy %.
The same substantially A-1 of A-4 Preparation of catalysts method, but the content difference of Pt, Re, Al.
The A-5 support of the catalyst is the SB bar, the same substantially A-1 of its preparation method, just the content difference of Pt, Re, Al.
The A-6 support of the catalyst also is the same substantially A-1 of SB bar its preparation method, just the content difference of Pt, Re, Al.
The catalyzer composition for preparing in this example sees Table 1, physicochemical property sees Table 2, Pt in the table 1, Re content X-ray fluorescence spectrometry, Ti content colorimetric method for determining, Al content and Re/Pt weight ratio are calculated value, and the specific surface in the table 2, pore volume, pore radius distribute and measure with static nitrogen loading capacity method.
Comparative Examples 1
This Comparative Examples does not contain the comparative catalyst of Al by prior art for preparing.
The D catalyzer is to be that carrier is by the Pt of commercial catalysts CB-6, the contrast medium that does not contain Al that Re content is made with the SB bar.
E is for being that carrier is by the Pt of commercial catalysts CB-7, the comparative catalyst who does not contain Al that Re content is made with the SB bar.
F is the not aluminiferous comparative catalyst who makes by A-4 Preparation of catalysts method in the disclosed example 4 of CN 1032951A.
The composition and the physicochemical property of D, E, F contrast medium are listed in table 1, the table 2 respectively.
Example 2
This example is the evaluation result on the pressurization micro-reactor for catalyzer of the present invention and industrial platinum-rhenium catalyst.
Used commercial catalysts B is Chang Ling refinery production, and industrial trade mark CB-7 contains the heavy % of Pt0.22, the heavy % of Re0.42, and rhenium platinum weight ratio is 2.0, and the used reaction raw materials of micro anti-evaluation is a normal heptane, and the appreciation condition of just living is 500 ℃, 9.8 * 10 5Pa, recovering the stage appreciation condition is 520 ℃, 9.8 * 10 5Pa, evaluation result sees Table 3, and wherein transformation efficiency refers to the normal heptane amount that transformed and the weight percent of the total input of normal heptane.The activity of catalyzer of the present invention as shown in Table 3 (A-1, A-2, A-3) and arenes selectivity all more do not contain catalyzer (3) height of Al.
Example 3
This example is catalyst A of the present invention-4 and the evaluation experimental of contrast medium F on the pressurization micro-reactor.
Used micro-reactor and raw material all with example 2, the results are shown in table 4, and as shown in Table 4, when rhenium platinum weight ratio was 1.0, catalyst activity of the present invention, selectivity were better than F, and (the used carrier of F is the HP ball, and its performance slightly is better than the SB ball.)
Example 4
This example is for the device of the 100 milliliters of hydrogen gas circulating systems evaluation experimental to catalyst A of the present invention-4 and industrial platinum-rhenium catalyst C (industrial trade mark CB-6, Chang Ling refinery).
Raw materials used oil is 70～150 ℃ of virgin naphthas, and oil property sees Table 5, and evaluation result sees Table 6, and appreciation condition is as follows:
Just live the stage: 480～520 ℃, 14.7 * 10 5Pa hydrogen/oil (body)=1200: 1
Air speed 2.0 hours -1
Accelerate the aging step: 540 ℃, 6.9 * 10 5Pa hydrogen/oil (body)=800: 1
Air speed 3.0 hours -1
The recovery stage: 500 ℃, 14.7 * 10 5Pa hydrogen/oil (body)=1200: 1
Air speed 2.0 hours -1
As shown in Table 6, catalyst A of the present invention-4 has activity and selectivity preferably, is recovering the stage transformation efficiency than catalyzer C high 1.5 heavy %, aromatics yield high 0.6 heavy %.The transformation efficiency method of calculation are as follows in the table 6:
Example 5
This example is activity and the selectivity contrast experiment of catalyst A of the present invention-5 with comparative catalyst D.
Used two catalyzer are that rhenium platinum weight ratio is 1.0 bar shaped catalyst, and stock oil is 80～160 ℃ of virgin naphthas, and oil property sees Table 7, and evaluation result sees Table 8, and evaluating apparatus is with example 4, and each stage appreciation condition is as follows:
Just live: 500～510 ℃ 15.0 * 10 5Pa hydrogen/oil (body)=1000: 1 air speed 2.0 hours -1
Accelerate aging: 530 ℃ 7.0 * 10 5Pa hydrogen/oil (body)=500: 1 air speed 2.0 hours -1
Recover: 520 ℃ 15.0 * 10 5Pa hydrogen/oil (body)=1000: 1 air speed 2.0 hours -1
Table 8 shows, catalyst A of the present invention-5 has higher activity and selectivity preferably, and stability slightly is better than contrast medium D.
Example 5
This example is the reactivity worth contrast experiment of catalyst A of the present invention-6 with comparative catalyst E.
Catalyst system therefor is bar shaped, and rhenium platinum weight ratio is 2.0.Raw materials used oil and appreciation condition are all with example 5, and evaluating apparatus is with example 4, and evaluation result is listed in table 9.Table 9 data show that equally catalyzer of the present invention has activity and selectivity preferably.
Table 1
The catalyzer numbering Catalyzer is formed (heavy %) Re/Pt (weight) Carrier
???Pt ???Re ???Al ???Ti
??A-1 ??0.21 ??0.40 ??0.01 ??0.10 ??1.90 The SB ball
??A-2 ??0.21 ??0.43 ??0.03 ??0.10 ??2.05 The SB ball
??A-3 ??0.21 ??0.41 ??0.05 ??0.10 ??1.95 The SB ball
??A-4 ??0.30 ??0.27 ??0.05 ??0.10 ??0.90 The SB ball
??A-5 ??0.25 ??0.27 ??0.06 ??0.10 ??0.96 The SB bar
??A-6 ??0.21 ??0.48 ??0.08 ??0.10 ??2.29 The SB bar
???D ??0.30 ??0.30 ??- ??0.10 ??1.00 The SB bar
???E ??0.21 ??0.45 ??- ??0.10 ??2.14 The SB bar
???F ??0.29 ??0.32 ??- ??0.14 ??1.10 The HP ball
Table 2
The catalyzer numbering Specific surface, rice 2/ gram Pore volume, milliliter/gram Can several apertures, Pore radius distributes, body %
??＜30 ??30～50 550～100 100～200 ?＞200
?A-1 ??189 ????0.45 ??82 ?????0 ??86.48 ??9.94 ??3.59 ??0
?A-2 ??185 ????0.50 ??82 ?????0 ??89.73 ??6.16 ??3.43 ?0.65
?A-3 ??185 ????0.50 ??82 ?????0 ??89.73 ??6.16 ??3.43 ?0.65
?A-4 ??188 ????0.48 ??82 ???4.0 ??90.90 ???5.0 ???0 ??0
?A-5 ??182 ????0.45 ??76 ??9.45 ??85.81 ??4.34 ??0.29 ?0.11
?A-6 ??185 ????0.46 ??67 ?22.53 ??75.22 ??1.23 ??0.32 ?0.11
??D ??182 ????0.45 ??76 ??9.45 ??85.81 ??4.34 ??0.29 ?0.11
??E ??185 ????0.46 ??67 ?22.53 ??75.72 ??1.23 ??0.32 ?0.11
??F ??195 ????0.58 ???- ????0 ??79.19 ?15.33 ??5.47 ??0
Table 3
Figure A9511645700121
Table 4
Reaction conditions The catalyzer numbering Reaction product, heavy %
Temperature, ℃ Pressure, handkerchief Cumulative time, hour ??C 1～C 5 Benzene and toluene Liquid yield
??500 ?9.8×10 5 ????1～2 ??A-4 ??21.23 ??14.52 ??78.77
????F ??22.55 ??11.86 ??77.45
??520 ?1.57×10 5 ????7 ??A-4 ??10.66 ??15.32 ??89.34
????F ??7.96 ??11.28 ??92.04
??520 ?9.8×10 5 ????8～9 ??A-4 ??17.55 ??11.64 ??82.45
????F ??18.56 ??10.70 ??81.44
Table 5
Proportion d 0 20 Boiling range, ℃ Hydrocarbon composition, heavy %
Initial boiling point ???10％ ????50％ ????90％ Do Alkane Naphthenic hydrocarbon Aromatic hydrocarbons Virtue is dived
0.7189 ????74 ????86 ????100 ????124 ????149 ?55.33 ??3.67 ??40.86 ??41.02
Table 6
Stage Temperature ℃ ????????????????????A-4 ??????????????????C
Liquid is received, heavy % Virtue contains, heavy % Virtue produces, heavy % Transformation efficiency, heavy % Liquid is received, heavy % Virtue contains, heavy % Virtue produces, heavy % Transformation efficiency, heavy %
Just live 480 ?86.1 ?49.92 ?43.0 ??105.3 ?85.1 ?49.72 ?42.3 ?103.5
520 ?75.0 ?61.19 ?51.9 ??126.9 ?73.3 ?69.97 ?51.3 ?125.5
Recover 500 ?90.9 ?47.66 ?43.3 ??106.0 ?89.8 ?49.61 ?42.7 ?104.5
Table 7
Boiling range, ℃ Hydrocarbon composition, heavy %
Initial boiling point ??10％ ???50％ ???90％ Do Alkane Naphthenic hydrocarbon Aromatic hydrocarbons Virtue is dived
??85 ???92 ???103 ???126 ???152 ?54.78 ?40.68 ?4.54 ?42.54
Table 8
Stage Temperature ℃ ????????????????????A-5 ???????????????????D
Liquid is received, heavy % Virtue contains, heavy % Virtue produces, heavy % Transformation efficiency, heavy % Liquid is received, heavy % Virtue contains, heavy % Virtue produces, heavy % Transformation efficiency, heavy %
Just live 500 ?82.4 ?62.0 ?51.1 ??121.1 ?82.1 ?61.2 ?50.3 ?118.2
510 ?79.7 ?67.8 ?54.1 ??127.0 ?79.7 ?67.7 ?54.0 ?126.9
Recover 510 ?87.2 ?55.2 ?48.2 ??113.3 ?86.4 ?55.5 ?47.9 ?112.6
Table 9
Stage Temperature ℃ ?????????????????A-6 ?????????????????????E
Liquid is received, heavy % Virtue contains, heavy % Virtue produces, heavy % Transformation efficiency, heavy % Liquid is received, heavy % Virtue contains, heavy % Virtue produces, heavy % Transformation efficiency, heavy %
Just live 510 ?75.6 ?76.40 ?57.7 ??135.6 ?74.9 ?75.80 ?56.9 ?133.8
Recover 520 ?80.0 ?69.70 ?55.6 ??130.7 ?79.9 ?68.50 ?54.7 ?128.6

Claims (10)

1. catalyst for reforming naphtha that contains metal Pt, Re, Ti and halogen is characterized in that having following composition (with the butt aluminum oxide is benchmark, heavy %):
Pt???0.10～1.00
Re???0.10～3.00
Ti???0.01～0.15
Al???0.01～0.15
Cl???0.50～3.00
γ-the Al of surplus 2O 3
2. according to the described catalyzer of claim 1, it is characterized in that having following composition (with the butt aluminum oxide is benchmark, heavy %):
Pt???0.10～0.50
Re???0.10～2.00
Ti???0.08～0.15
Al???0.01～0.08
Cl???0.50～1.50
γ-the Al of surplus 2O 3
3. according to claim 1 or 2 described catalyzer, it is characterized in that described Al form with unformed aluminum oxide in catalyzer exists.
4. according to claim 1 or 2 described catalyzer, it is characterized in that described γ-Al 2O 3High-purity γ-the Al that gets for alkyl aluminum hydrolysis 2O 3
5. according to claim 1 or 2 described catalyzer, it is characterized in that rhenium platinum weight ratio is 0.5～4.0.
6. according to the described catalyzer of claim 4, it is characterized in that rhenium platinum weight ratio is 1.0～3.0.
7. according to claim 1 or 2 described catalyzer, it is characterized in that this catalyzer can make with the method for the common impregnated carrier of precursor of each metal constituent element of usefulness of routine, also the method for available step impregnation makes.
8. according to the described catalyzer of claim 7, the precursor that it is characterized in that Al is aluminum nitrate or aluminum chloride, preferably AlCl 3
9. according to the described catalyzer of claim 7, it is characterized in that the Ti constituent element can be introduced directly in the carrier with coprecipitation method in the preparing carriers process.
10. claim 1 or 2 described catalyzer are used for the coking that boiling range is 40～230 ℃ virgin naphtha or its blending refining of petroleum, the boiling range that cracking technology is produced is the reforming process of 40～230 ℃ gasoline, are specially adapted to the reformation of virgin naphtha.
CN95116457A 1995-10-06 1995-10-06 Multiple-metal reforming catalyst Expired - Lifetime CN1039818C (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101294102B (en) * 2007-04-28 2011-06-15 中国石油化工股份有限公司 Petroleum naphtha reforming catalyst and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN100344373C (en) * 2004-08-31 2007-10-24 中国石油化工股份有限公司 Multi-metal reforming catalyst and preparing method

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US4305810A (en) * 1980-10-02 1981-12-15 Atlantic Richfield Company Stabilized reforming catalyst
CN1015636B (en) * 1987-11-04 1992-02-26 中国石油化工总公司石油化工科学研究院 Naphtha reforming catalyst
CN1015637B (en) * 1988-02-25 1992-02-26 中国石油化工总公司石油化工科学研究院 Beta zeolite-containing hydrocarbon reforming catalyst
CN1020378C (en) * 1990-03-17 1993-04-28 中国石油化工总公司 Catalyst for reforming naphtha
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101294102B (en) * 2007-04-28 2011-06-15 中国石油化工股份有限公司 Petroleum naphtha reforming catalyst and preparation method thereof

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