CN101885980B - Preparation method and application of catalytic cracking metal passivant - Google Patents
Preparation method and application of catalytic cracking metal passivant Download PDFInfo
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Abstract
The invention relates to a preparation method and application of a catalytic cracking metal passivant. The preparation method comprises the following steps of: preparing raw materials in the following percentage by weight: 20%-45% of dispersing agents, 30%-50% of oxidants, 15%-30% of metal oxides, 10%-30% of solvents and 2%-5% of stabilizing agents; sequentially adding the oxidants and the metal oxides to the dispersing agents during preparation; increasing temperature to 50-90 DEG C within 2-4 hours, keeping the temperature for 1-5 hours and then cooling; adding the solvents and the stabilizing agents, and then filtering to remove impurities so as to obtain the metal passivant, wherein the dispersing agents are diethanol amine and/or triethanol amine; the oxidants are hydrogen peroxide of 30-50 percent and/or nitric acids of 66-68 percent; the metal oxides are one of diantimony trioxide, rare earth oxides and bismuth oxides or mixtures of more than two of the diantimony trioxide, the rare earth oxides and the bismuth oxides in any proportion; the solvents are one of water or alcohol solvents or mixtures of more than two of the water or the alcohol solvents in any proportion; and the stabilizing agents are methylcellulose compound solutions.
Description
Technical field
The present invention relates to a kind of preparation method and application thereof of catalytic cracking metal passivant.
Background technology
CCU has occupied dominant position in oil refining apparatus, raw material through after the heat exchange with catalyst cracker in catalyzer contact cracking, obtain dry gas, liquefied gas, gasoline, diesel oil, coke and slurry oil.Receive the influence of oil supply and quality; Metal element content in the crude oil increases day by day; Each oil refinery company is pursued is high intermingled dregs ratio, lower coking yield and high lightweight oil or total liquid yield; To reach maximum economic benefits, also quickened the metallic element in the fcc raw material from another point of view and risen.Metallic element in the fcc raw material is very large for the harm of catalyzer, and particularly nickel is particularly serious to catalyzer harm, thereby can influence the distribution of catalytic cracking product.At home and abroad, have many about improving the method report that the catalytic cracking product distributes.
CN1245198A has reported the preparation method who contains antimony metal passivator, with weisspiessglanz, organic carboxyl acid, aliphatic amide and water, under 80～180 ℃, has synthesized water-soluble metal passivator in this method.Dominant mechanism is in raw material, to add antimony containing compounds, and passivation nickel is to the influence of catalytic cracking catalyst.One is one or more mixtures of compounds such as water-soluble antimony, rare earth, tin metal passivator in the device of FCC (hereinafter to be referred as FCC) at present; Its shortcoming is to be prone under the low temperature separate out; Decomposition temperature is low, poorly soluble in raw oil, and dispersing property is bad.And one requires the effective metal antimony content more than 15% in the product.
CN10121A5476A has reported a kind of preparation method and industrial application of assistant for catalytic cracking coking-inhibiting yield-increasing; In 1～3 hour, be warmed up to 50～150 ℃ with oil-soluble dispersant, thermo-cracking promoting agent, radical chain reaction suppressor factor, oil soluble metal passivator, varsol in this method; Be incubated 1～5 hour, the cooled and filtered removal of impurity promptly gets the coking-inhibiting yield-increasing auxiliary agent.Major function improves intermingled dregs ratio, the raising yield of light oil of FCC apparatus and reduces coke yield, and can reduce the consumption of device metal passivator or stop annotating metal passivator, improves the overall efficiency of FCC apparatus.This product only can be at part CCU alternative metals passivator, and is invalid basically for the heavy metal contamination of MIP-CGP (voluminous isoparaffin and propylene enhancing) technology CCU.
Summary of the invention
The present invention provides a kind of preparation method of catalytic cracking metal passivant, and the gained catalytic cracking metal passivant can improve the pollution capacity of the preventing from heavy metal nickel of CCU, reduces the green coke productive rate and improves yield of light oil.
The present invention also provides the application of the catalytic cracking metal passivant that above-mentioned preparation method obtains.
The preparation method of said catalytic cracking metal passivant does; Proportioning raw materials is: dispersion agent 20%～45%, oxygenant 30%～50%, MOX 15%～30%, solvent 10%～30%, and stablizer 2%～5%, said per-cent is mass percent; During the preparation catalytic cracking metal passivant; In dispersion agent, add oxygenant, MOX successively, in 2～4 hours, be warmed up to 50～90 ℃, be incubated 1～5 hour; Cooling adds the solvent and the removal of impurity of stablizer after-filtration and promptly gets metal passivator;
Wherein,
Said dispersion agent is diethylolamine and/or trolamine, is preferably trolamine;
Said oxygenant is that mass percent concentration is that 30%～50% ydrogen peroxide 50 and/or mass percent concentration are 66%～68% nitric acid, is preferably mass percent concentration and is 30%～50% ydrogen peroxide 50;
Said MOX is the mixture of one or more arbitrary proportions in Antimony Trioxide: 99.5Min, rare earth oxide, the bismuth oxide compound, is preferably the mixture of Antimony Trioxide: 99.5Min or Antimony Trioxide: 99.5Min and rare earth oxide.Rare earth oxide is preferably cerium oxide and/or lanthanum trioxide.For MOX is the situation of mixture, and the preferred wherein mass percentage content of Antimony Trioxide: 99.5Min is 70%～80%;
Said solvent is the mixture of one or more arbitrary proportions in water or the alcoholic solvent, the mixture of one or more arbitrary proportions in preferably water, terepthaloyl moietie, the USP Kosher, more preferably terepthaloyl moietie and/or USP Kosher;
Said stablizer is the mixture of one or more any ratios in the methylcellulose gum compounds solution; Cmc soln more preferably; The substitution value of said CMC 99.5 is 0.65～0.85; The polymerization degree is 200～1000, and said solution is that mass percent concentration is 2%～5% the aqueous solution.
As preferred version of the present invention; Proportioning raw materials is: dispersion agent 30～40%, oxygenant 40～50%, MOX 15～30%, solvent 10～15%, stablizer 2%～5%; Wherein, the consumption of MOX more preferably 19～21%, the consumption of solvent more preferably 10～12%, the consumption of stablizer more preferably 2%～3%.
Gained catalytic cracking metal passivant of the present invention directly joins in the catalytically cracked material; Dispersed good in fcc raw material, when using above-mentioned catalytic cracking metal passivant, addition is 10～80ppm of catalytically cracked stock weight; Be preferably 15～60ppm, most preferably be 20～30ppm.
After nickel compound in the raw oil decomposed in reactor drum, one formed nickel oxide, also had the nickel of 0 valency and+1 valency; Nickel is with+2 in revivifier, and+3 valency forms exist.The form of nickel mainly is nickel oxide, nickel aluminate or silicoaluminate nickel; Nickel can be evenly dispersed on the catalyzer; Have stronger dehydrogenation activity, so nickel poisoning causes the dehydrogenation activity rising of catalyzer, coke, dry gas and hydrogen yield increase; Light oil yield descends, but nickel is less to the activity of such catalysts influence.
According to the nickel suppressor factor of nickel poisoning mechanism design, one is to adopt the compound of metallic elements such as antimony, bismuth and Sb-Ni or the Bi-Ni alloy that nickel forms larger particles, stops the dispersion of nickel, thereby reaches the active purpose that reduces nickel.
Synthetic metal passivator of the present invention contains the high price sb oxide, has the heat decomposition temperature height, hangs the high advantage of antimony rate, under the catalysis system condition, preferentially combines with nickel, thereby it is lost dehydrogenation activity and good stability, is difficult for being reduced.Through in fcc raw material, adding a small amount of gained metal passivator of the present invention; Dispersion agent wherein can change the surface properties of raw oil, reduces its viscosity and surface tension, thereby improves the atomization of catalytically cracked material; Reduce fogdrop diameter; Shorten the gasification time, improve the velocity of diffusion of oil gas molecule on catalyzer, reduce the generation of condensation reaction and hydrogen transfer reactions; The mixture of high price sb oxide wherein or high price antimony and cerium can improve the character of equilibrium catalyst; The Lewis acid (L acid) that generates the aluminum oxide of from framework of molecular sieve, constantly deviating from is converted into Blang's acid (B acid); Suppress the burnt generation of catalysis, effectively passivation harmful heavy metal (Ni-V-Fe, sodium etc.).
Advantage such as the present invention has the stable performance of decomposition temperature high and low temperature, dispersing property is good in raw oil; And effective metal content high (content one more than 15%); Under the constant situation of raw oil, effectively reduce hydrogen and methane ratio in the dry gas, increase total liquid and receive.
Through 1,000,000 tons of/year technology heavy oil catalytically cracking equipments (MIP-CGP technology) industrial test; Test-results shows that the present invention is under the situation of raw oil character variation and heavy metal content increase; Hydrogen that can assurance device does not increase than with methane; The productive rate of coke does not rise simultaneously, descends 0.2% on the contrary, and total liquid is received and increased more than 0.5%.In the CCU raw material, add the present invention, can improve the preventing from heavy metal pollution ability of device, reduce coke yield and the liquid yield that improves device, simple to operate, the auxiliary agent cost is low, the remarkable in economical benefits of device.
Embodiment
Further specify content of the present invention below in conjunction with embodiment.
In following examples, the substitution value of used CMC 99.5 is 0.65～0.85, and the polymerization degree is 200～1000.
Embodiment 1
Earlier diethylolamine 1000kg is joined in the stainless steel cauldron; In 1 hour, be warmed up to 70～90 ℃, stir, add ydrogen peroxide 50 2300kg, Antimony Trioxide: 99.5Min 1000kg successively; Be incubated 1～5 hour; After oxidizing reaction finished, cooling added terepthaloyl moietie 500kg, CMC 99.5 (2% the aqueous solution) 100kg stirs and filtering and impurity removing matter promptly gets water-soluble metal passivator A.
Embodiment 2
Earlier trolamine 1500kg is joined in the stainless steel cauldron; In 1 hour, be warmed up to 70～90 ℃; Stir, add ydrogen peroxide 50 1600kg, Antimony Trioxide: 99.5Min 800kg, cerium oxide 100kg, lanthanum trioxide 100kg, 68% nitric acid 300kg insulation 1～5 hour successively, after oxidizing reaction finishes; Cooling adds USP Kosher 500kg, CMC 99.5 (2% the aqueous solution) the 100kg filtering and impurity removing matter that stirs and promptly gets water-soluble metal passivator B.
Embodiment 3
Earlier diethylolamine 1000kg, trolamine 900kg are joined in the stainless steel cauldron; In 1 hour, be warmed up to 70～90 ℃, stir, add ydrogen peroxide 50 1500kg, Antimony Trioxide: 99.5Min 1000kg successively; Be incubated 1～5 hour; After oxidizing reaction finished, cooling added terepthaloyl moietie 300kg, USP Kosher 200kg, CMC 99.5 (2% the aqueous solution) the 100kg filtering and impurity removing matter that stirs and promptly gets water-soluble metal passivator C.
Embodiment 4
Earlier trolamine 1500kg is joined in the stainless steel cauldron; In 1 hour, be warmed up to 70～90 ℃, stir, add ydrogen peroxide 50 1700kg, Antimony Trioxide: 99.5Min 700kg, cerium oxide 200kg, bismuth oxide 100kg successively; 68% nitric acid 200kg insulation 1～5 hour; After oxidizing reaction finished, cooling added terepthaloyl moietie 500kg, CMC 99.5 (2% the aqueous solution) the 100kg filtering and impurity removing matter that stirs and promptly gets water-soluble metal passivator D.
Embodiment 5
This test is the fixed fluidized bed FCC tests device that certain catalyzer Ltd buys from Research Institute of Petro-Chemical Engineering of Sinopec Group at the device that adopts; Water-soluble metal passivator A, B, C, D are carried out Simulation evaluation, and the consumption of metal passivator is the 60ppm of raw oil quality.Experiment parameter and result are shown in table 1-5.
Can be found out the water-soluble metal passivator of interpolation 60ppm in fcc raw material by table 1-5 after, the hydrogen in the dry gas has descended 24% with the methane ratio, and total liquid yield increases about 1%.
Table 1, raw oil main character
Table 2, equilibrium catalyst main character (the catalyzer model is DOCO)
| Project | Character |
| Settled density: the g/mL iron content: ppm contains vanadium: ppm is nickeliferous: the little index alive of ppm: % | 0.83 3500 1160 14100 58.7 |
The analysis of table 3 test sample typical case performance perameter
Table 4 material balance
| Test number | 0 # | 1 # | 2 # | 3 # | 4 # |
| Test period | 2007.5.20 | 2007.5.27 | 2007.6.5 | 2007.6.10 | 2007.7.15 |
| Raw oil | Raw oil | Raw oil+A | Raw oil+B | Raw oil+C | Raw oil+D |
| Catalyzer | Poiser | Poiser | Poiser | Poiser | Poiser |
| Temperature of reaction, ℃ | 505 | 505 | 505 | 505 | 505 |
| Agent-oil ratio (?) | 6 | 6 | 6 | 6 | 6 |
| Air speed, l/h | 15 | 15 | 15 | 15 | 15 |
| Material balance, m% | |||||
| Dry gas | 3.5 | 3.2 | 3.2 | 3.2 | 3.1 |
| Gasoline+diesel oil | 66.6 | 69.2 | 69.3 | 69.1 | 69.1 |
| Liquefied gas+gasoline+diesel oil | 85.2 | 87.3 | 87.2 | 87.3 | 87.3 |
| Heavy oil+coke | 10.6 | 8.9 | 9.1 | 9.0 | 9.0 |
| Loss, m% | 0.7 | 0.6 | 0.5 | 0.5 | 0.6 |
| Amount to | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 |
Table 5 takes off preceding dry gas component MV
| Test number | 0 # | 1 # | 2 # | 3 # | 4 # |
| Test period | 2004.8.31 | 2004.9.1 | 2004.9.2 | 2004.9.4 | 2004.9.5 |
| Raw oil | Heavily urge raw oil | Raw oil+A | Raw oil+B | Raw oil+C | Raw oil+D |
| Catalyzer | Poiser | Poiser | Poiser | Poiser | Poiser |
| Temperature of reaction, ℃ | 505 | 505 | 505 | 505 | 505 |
| Agent-oil ratio | 6 | 6 | 6 | 6 | 6 |
| Air speed, l/h | 15 | 15 | 15 | 15 | 15 |
| Dry gas is formed, V% | |||||
| Methane | 25.4 | 29 | 27 | 28 | 27 |
| Hydrogen | 36.6 | 31 | 30 | 30.4 | 30 |
| Other | 38 | 40 | 43 | 41.6 | 43 |
| Hydrogen first ratio | 1.44 | 1.06 | 1.11 | 1.09 | 1.11 |
Embodiment 6
Embodiment 2 said water-soluble metal passivator B carry out industrial application experiment (before the agent of the present invention of annotating at the water-soluble metal passivator with domestic certain auxiliary agent company) at 1,000,000 tons of/year RFCCs of certain refinery; Joining day is that March 1 was to March 25; Amount to 25 days, add-on is 60PPm/kg (raw material).Between the usage period, other main operating parameters and the feedstock property of device remain unchanged.Take off H in the preceding dry gas before and after using the present invention
2/ CH
4Changing conditions is seen table 6.
Can find out by table 6: after the device trial edition invention, before taking off in the dry gas volume ratio of hydrogen and methane occur significantly descending, and the same period live catalyst consumption slightly reduce, show that this agent effect aspect the dehydrogenation of inhibition heavy metal is better.
Embodiment 7
Embodiment 3 said water-soluble metal passivator C carry out industrial performance test at Sinopec branch office 2,800,000/year heavy-oil catalytic device (MIP-CGP technology); The intermingled dregs ratio of this device reaches 75%; Heavy metal content high (Ni+V MV is up to 13.7ppm) in the residual oil at the water-soluble metal passivator with domestic certain auxiliary agent company, adds agent front and back processing condition and remains unchanged before the agent of the present invention of annotating; 4.24～5.1 is the quick adding phase; Add-on is 50ppm (to a raw oil), and 5.1 begin to balance adds the phase, and add-on is 30ppm (to a raw oil).Add the forward and backward feedstock property of agent and change and see table 7, add the forward and backward material balance of agent and see table 8, add in the forward and backward dry gas of agent each change of component situation and see table 9.Wherein, the data that add after the agent are to record the balance adding phase.
Can be found out by table 7: raw oil character becomes heavy before and after adding agent, and density increases, carbon residue is increased to 6.19 by 5.82, and heavy metal content increases.
Can be found out by table 8: become under the situation about weighing at raw oil, add before and after the agent, device is found out from material balance; The slurry oil yield obviously descends; Light liquid is received slightly and is risen, and the raising owing to catalyst activity is described, the cracking ability rises; But cause fcc raw material to change greatly because oil variety is changed, thereby cause green coke obviously slightly to rise.
Table 6: MV in the dry gas before live catalyst consumes situation and takes off before and after using
| Project | Before using (on February 1 to 25) | Use back (on March 1 to 25) |
| Catalyst consumption | 112 tons | 111 tons |
| Catalyst consumption | 1.52kg/t raw material | 1.43kg/t raw material |
| Dry gas H before taking off 2 | 36.6 | 30.4 |
| Dry gas CH before taking off 4 | 25.4 | 28 |
| H 2/CH 4 | 1.44 | 1.08 |
Table 7: feedstock property
Table 8: material balance
Table 9: each change of component situation in the dry gas before taking off
| Project | Before the filling | After the filling |
| H 2 | 29.01 | 26.32 |
| CH 4 | 20.33 | 21.58 |
| CO | 0.82 | 1.77 |
| C 2H 6 | 10.28 | 10.48 |
| C 2H 4 | 12.42 | 12.86 |
| CO 2 | 3.84 | 4.27 |
| C 3H 8 | 0.26 | 0.27 |
| C 3H 6 | 1.29 | 1.33 |
| iC 4H 10 | 0.14 | 0.15 |
| nC 4H 10 | 0.03 | 0.02 |
| nC 4H 8 | 0.03 | 0.03 |
| iC 4H 8 | 0.05 | 0.04 |
| tC 4H 8 | 0.03 | 0.03 |
| cC 4H 8 | 0.02 | 0.02 |
| ≥C 5 | 0.03 | 0.04 |
| H 2S | 0.32 | 0.29 |
| N 2 | 14.62 | 13.95 |
| ≥C6 | 0.01 | 0.01 |
| H/CH4 | 1.43 | 1.22 |
Can find out from embodiment 5-7: metal passivator passivation effect of the present invention is remarkable, can reduce hydrogen/methane value in the catalytic cracked dry gas effectively, improves total liquid of device and receives, and filling is convenient, can improve the whole economic efficiency of CCU.
Claims (7)
1. the preparation method of a catalytic cracking metal passivant; It is characterized in that proportioning raw materials is: dispersion agent 20%～40%, oxygenant 30%～50%, MOX 15%～30%, solvent 10%～30%, stablizer 2%～5%; Said per-cent is mass percent; During the preparation catalytic cracking metal passivant, in dispersion agent, add oxygenant, MOX successively, in 2～4 hours, be warmed up to 50～90 ℃; Be incubated 1～5 hour, the cooling back adds solvent and stablizer filtering and impurity removing matter promptly gets metal passivator;
Wherein,
Described dispersion agent is diethylolamine and/or trolamine;
Said oxygenant is that mass percent concentration is that 30%～50% ydrogen peroxide 50 and/or mass percent concentration are 66%～68% nitric acid;
Said MOX is the mixture of one or more arbitrary proportions in Antimony Trioxide: 99.5Min, rare earth oxide, the bismuth oxide compound;
Said solvent is the mixture of one or more arbitrary proportions in water or the alcoholic solvent;
Said stablizer is the mixture of one or more any ratios in the methylcellulose gum compounds solution.
2. the preparation method of catalytic cracking metal passivant as claimed in claim 1 is characterized in that, proportioning raw materials is: dispersion agent 30～40%, oxygenant 40～50%, MOX 15～30%, solvent 10～15%, stablizer 2%～5%.
3. according to claim 1 or claim 2 the preparation method of catalytic cracking metal passivant is characterized in that said oxygenant is that mass percent concentration is 30%～50% ydrogen peroxide 50.
4. according to claim 1 or claim 2 the preparation method of catalytic cracking metal passivant is characterized in that said MOX is Antimony Trioxide: 99.5Min and/or cerium oxide.
5. according to claim 1 or claim 2 the preparation method of catalytic cracking metal passivant is characterized in that said solvent is terepthaloyl moietie and/or USP Kosher.
6. according to claim 1 or claim 2 the preparation method of catalytic cracking metal passivant; It is characterized in that; Said stablizer is a cmc soln; The substitution value of said CMC 99.5 is 0.65～0.85, and the polymerization degree is 200～1000, and said solution is that mass percent concentration is 2%～5% the aqueous solution.
7. the application of each said catalytic cracking metal passivant in the claim 1～6 is characterized in that addition is 15～60ppm of catalytically cracked stock weight.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102229813B (en) * | 2011-05-23 | 2013-07-17 | 陕西超能石化科技有限公司 | Multifunctional desulphurization auxiliary agent of distillate of FCC device and preparation method thereof |
| CN103055916B (en) * | 2011-10-21 | 2015-06-17 | 中国石油化工股份有限公司 | Preparation method of catalytic cracking catalyst |
| CN102660317B (en) * | 2012-05-24 | 2014-04-16 | 沧州信昌化工有限公司 | Auxiliary for increasing yield of light oil in oil catalytic cracking device, and preparation method of auxiliary |
| CN102974403A (en) * | 2012-12-11 | 2013-03-20 | 江苏汉光实业股份有限公司 | Catalytic-cracking metal passivator |
| CN102974399A (en) * | 2012-12-11 | 2013-03-20 | 江苏汉光实业股份有限公司 | Preparation method of catalytic cracking metal deactivator |
| CN103285937A (en) * | 2013-05-22 | 2013-09-11 | 吴江市德佐日用化学品有限公司 | Catalytic cracking metal passivator and preparation method thereof |
| CN104162455A (en) * | 2014-07-02 | 2014-11-26 | 宜兴汉光高新石化有限公司 | A water-soluble catalytic cracking multifunctional deactivator and a preparing method thereof |
| CN106475155B (en) * | 2015-08-28 | 2019-09-20 | 江苏科创石化有限公司 | A kind of matal deactivator and preparation method thereof |
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