CN100410351C - Method for removing powder of catalyst in catalytic cracking oil slurry - Google Patents
Method for removing powder of catalyst in catalytic cracking oil slurry Download PDFInfo
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- CN100410351C CN100410351C CNB200510116841XA CN200510116841A CN100410351C CN 100410351 C CN100410351 C CN 100410351C CN B200510116841X A CNB200510116841X A CN B200510116841XA CN 200510116841 A CN200510116841 A CN 200510116841A CN 100410351 C CN100410351 C CN 100410351C
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Abstract
This invention provides two methods for removing catalyst powder from catalytic cracking oil slurry. The first method is suitable for light oil slurry whose specific gravity is lower than water, and comprises: mixing water containing demulsifier and flocculant with catalytic cracking oil slurry, demulsifying and removing the lower layer of water enriched in catalyst powder. The second method is suitable for heavy oil slurry whose specific gravity is higher than water, and comprises: adding weak electrolyte or non-electrolyte that can be dissolved in water and has higher specific gravity into water, such as ammonium acetate, ammonium citrate, fructose, glucose, sucrose, sorbitol or xylitol. The two methods have such advantages as short removing time and high rate.
Description
Technical field
The present invention relates to the process for purification of hydrocarbon ils, exactly, is the method that removes catalyst fines in the catalytically cracked oil.
Background technology
Catalytically cracked oil (be called for short FCC slurry oil) is in the catalytic cracking process, and the unconverted hydro carbons of boiling point＞350 ℃ wherein is rich in colloid, and bituminous matter has the viscosity height, the characteristics that density is big.The FCC slurry oil is mainly used in the blend component of heavy fuel oil (HFO), and hydrocracking raw material is produced carbon black, needle coke, and rubber and plastic processing aid.Be rich in the solid catalyst powder in the FCC slurry oil, ash content is higher, generally at (0.2-0.9wt%).Catalyst fines can have influence on the quality of derived product, and during for example as carbon black and needle-shape coke raw material, ash content is necessary＜0.05wt%, the top grade product are then wanted＜0.02wt%.In addition, the slurry oil that is rich in catalyst fines can quicken the wearing and tearing of nozzles when making the oil fuel component, can the blocking catalyst duct when making hydrocracking raw material, increase pressure drop.So must take measures, remove the solid catalyst powder in the FCC slurry oil.
The existing technology that removes comprises: natural subsidence, electrostatic separation, centrifugal separation etc. are filtered in the auxiliary agent sedimentation.Natural subsidence is the method for using the earliest, because the particle size range of catalyst fines is at 0-80 μ m, wherein the following particle diameter of 20 μ m accounts for suitable proportion, settling velocity is slow, and slurry oil viscosity is big, has hindered the sedimentation of catalyst fines, even so elevated temperature, effect of settling is also undesirable.Filter, electrostatic adhesion is separated, and methods such as centrifugation are all very high to equipment requirements.Filtration unit requires the small-sized of filter opening, thereby is easy to stop up back flushing continually; The electrostatic adhesion tripping device is wrapped up by oil owing to solid surface and can not reach ideal effect; Centrifugation is owing to the large batch of slurry oil of intractable, so do not have examples of industrial applications.At the shortcoming of natural subsidence, many bibliographical informations the interpolation auxiliary agent quicken settled method.Auxiliary agent is some surfactants normally, as: alkylphenol-formaldehyde resin and alkoxyl group polyacrylic acid affixture, unsaturated fatty acids, alkyl benzene sulphonate (ABS) etc.USP5,481,059 introduce vinylformic acid and resol alkoxylate affixture is made settling aids, USP5,593,572 introduce with containing N, S, heteroatomic aliphatic polymer such as O make settling aids (molecular weight 103-106), USP5,681,451 introductions are made auxiliary agent with the alkoxylated alkylphenol urea formaldehyde of molecular weight 1500-5000, USP6,316,685 introduce with containing polyvalent alcohol, and the unitary unsaturated carboxylic acid polymer of alkoxide alkyl phenolic resin is made settling aids.The auxiliary agent sedimentation can improve effect of settling greatly and shorten the settling time, even yet like this, settling time also will be about 24 hours even several days, and catalyst fines is enriched in the slurry oil of container bottom, also will remove catalyst fines and reclaim slurry oil through means such as filtration and centrifugations, these all have influence on treatment capacity and processing cost.
Summary of the invention
The invention provides two kinds of methods that remove catalyst fines in the catalytically cracked oil, these two kinds of methods are short to the time that removes of catalyst fines, the decreasing ratio height.
First kind of method that removes catalyst fines in the catalytically cracked oil provided by the invention, be applicable to and handle the lightweight slurry oil of proportion less than water, this method comprises: the water that will contain emulsion splitter and flocculation agent mixes with catalytically cracked oil, breakdown of emulsion, with enrichment the lower layer of water of catalyst fines tell and get final product.
In order to guarantee mixed effect, mix after water and catalytically cracked oil are preheating to 95-100 ℃ respectively, at 90-140 ℃ of following heating demulsification type, or under the 2000-5000v/cm electric field breakdown of emulsion.
The water yield is the heavy % of the 5-30 of catalytically cracked oil weight, preferably the heavy % of 10-20.
The effect of emulsion splitter is that the water sepn in the mixture is come out, and emulsion splitter can be that alkoxylated alkylphenol urea formaldehyde, polyvalent alcohol polyoxyethylene polyoxypropylene block copolymer, polyethylene polyamine polyoxyethylene polyoxypropylene block copolymer and compound thereof and all are applicable to the commercially available emulsion splitter of slurry oil breakdown of emulsion.The emulsion splitter dosage is the 10-500ppm of the weight of slurry oil, preferably 20-100ppm.
Flocculation agent is inorganic or organic polymer, as polymerization silicate, poly-ferric chloride, polymerize aluminum chloride, Poly Dimethyl Diallyl Ammonium Chloride, polyacrylamide, sodium polyacrylate, acrylic acid-acrylamide copolymer etc., and all are applicable to the settled commercially available flocculation agent of catalyst fines.The consumption of flocculation agent is the 10-1000ppm of slurry oil weight, preferably 200-1000ppm.
Second kind of method that removes catalyst fines in the catalytically cracked oil provided by the invention, be applicable to and handle the heavy slurry oil of proportion more than or equal to water, this method comprises: the water that will contain weighting agent, emulsion splitter and flocculation agent mixes with catalytically cracked oil, breakdown of emulsion, with enrichment the lower layer of water of catalyst fines tell and get final product.
In order to guarantee mixed effect, water and catalytically cracked oil are preheating to 95-100 ℃.Mix the back under 90-140 ℃, add 2000-5000v/cm electric field breakdown of emulsion.
The water yield is the heavy % of the 5-30 of catalytically cracked oil weight, preferably the heavy % of 10-20.
Said weighting agent is the material that can increase the proportion of water, and promptly proportion is greater than water and weak electrolyte or the nonelectrolyte miscible with water, as: ammonium acetate, ammonium citrate, fructose, glucose, sucrose, sorbyl alcohol, Xylitol etc.The consumption of weighting agent should make the proportion of the proportion of the water that contains weighting agent greater than catalytically cracked oil, the heavy % of the 5-30 that general consumption is a water weight, the preferably heavy % of 10-20.
The effect of emulsion splitter is that the water sepn in the mixture is come out, and emulsion splitter can be alkoxylated alkylphenol urea formaldehyde, polyvalent alcohol polyoxyethylene polyoxypropylene block copolymer, polyethylene polyamine polyoxyethylene polyoxypropylene block copolymer and compound thereof.And all are applicable to the commercially available emulsion splitter of slurry oil breakdown of emulsion.The emulsion splitter dosage is the 10-500ppm of the weight of slurry oil, preferably 20-100ppm.
Flocculation agent is inorganic or organic polymer, as polymerization silicate, poly-ferric chloride, polymerize aluminum chloride, Poly Dimethyl Diallyl Ammonium Chloride, polyacrylamide, sodium polyacrylate, acrylic acid-acrylamide copolymer etc., and all are applicable to the settled commercially available flocculation agent of catalyst fines.The consumption of flocculation agent is the 10-1000ppm of slurry oil weight, preferably 200-1000ppm.
In order to improve removal effect, two kinds of methods provided by the invention all can adopt second-stage treatment, and the slurry oil that is about to after one-level is handled is handled once according to the method described above again.Separate the water of discharging, through sedimentation, the catalyst powder that removes by filter suspension is last, and is reusable.Reusable water need not to add the material that increases proportion again when handling the heavy slurry oil, and the amount of emulsion splitter and flocculation agent also can suitably reduce.
Two kinds of methods provided by the invention can be respectively applied for handles proportion less than the lightweight slurry oil of water and the proportion heavy slurry oil more than or equal to water, and it is short that catalyst fines is removed the time, and the decreasing ratio height can make ash content reach requirement after taking off.
Embodiment
Removal effect among the embodiment assigns to estimate with ash, and the measuring method of ash content is seen GB508-65, get at every turn take off before slurry oil contrast the calculating of decreasing ratio.
Embodiment 1
The character of the slurry oil A that handles sees Table 1.Flocculation agent dosage 1000ppm, emulsion splitter (FC9301) dosage 100ppm, concrete grammar is as follows: in 15.2g water, add 0.8g emulsion splitter (concentration 2 heavy %), and mix wiring solution-forming with 16g flocculation agent (concentration 1 heavy %), after being preheating to 95 ℃, mix with the 160g slurry oil that is preheating to 100 ℃ in advance, click to mix 50 times with juice extractor, fall in test tube added electric field in the breakdown of emulsion instrument, leave standstill breakdown of emulsion and divide water, strength of electric field 2000v/cm, take out after 1 hour, extract lower layer of water out, get the slurry oil survey ash content that stirs.Test-results sees Table 2, and the removal effect of polyacrylamide is best, and taking off back slurry oil ash content is 0.01%, decreasing ratio 95.2%.
The character of table 1 catalytically cracked oil A
The removal effect of the different flocculation agents of table 2
Embodiment 2
The character of the slurry oil A that handles sees Table 1.Adopt the not method of the hot breakdown of emulsion of added electric field, flocculation agent is selected polyacrylamide for use, dosage 1000ppm, emulsion splitter (FC9301) dosage 100ppm, concrete grammar is as follows: in 15.2g water, add 0.8g emulsion splitter (concentration 2 heavy %), and mix wiring solution-forming with 16g flocculation agent (polyacrylamide, 1 heavy % concentration), be preheating to 95 ℃ after, mix with the 160g slurry oil that is preheating to 100 ℃ in advance, click mixing 50 times with juice extractor, place the pressurized vessel heating demulsification type, take out after 2 hours, extract lower layer of water out, get the slurry oil survey ash content that stirs.Test-results sees Table 3, under same temperature condition, the denitrating catalyst powder effect of hot breakdown of emulsion is than the added electric field weak effect, 95 ℃ decreasing ratio is 89.1%, along with temperature raises, improved the effect of oily water separation, decreasing ratio is also along with rising, 125 ℃ decreasing ratio is 94.2%, near the effect of electric field breakdown of emulsion.
The removal effect of the different settling temperature of table 3
Embodiment 3
The character of the slurry oil B that handles sees Table 4.Increase the proportion of water with sucrose, flocculation agent dosage 1000ppm, emulsion splitter (FC9301) dosage 100ppm, concrete grammar is as follows: get 6.4g sucrose and add in the 15.2g water, add 0.8g emulsion splitter (concentration 2 heavy %), and mix wiring solution-forming with 16g flocculation agent (concentration 1 heavy %), after being preheating to 95 ℃, mix, click with juice extractor and mix 50 times with the 160g slurry oil that is preheating to 100 ℃ in advance, fall in test tube added electric field in the breakdown of emulsion instrument, leave standstill breakdown of emulsion and divide water, strength of electric field 2000v/cm took out after 1 hour, extract lower layer of water out, get the slurry oil survey ash content that stirs.Test-results sees Table 5, from table data as can be seen, the polyacrylamide effect is best, decreasing ratio reaches 87.4%, taking off back slurry oil ash content is 0.0419%.
The character of table 4 catalytically cracked oil B
The removal effect of the different flocculation agents of table 5
Embodiment 4
The character of the slurry oil B that handles sees Table 4.Increase proportion with glucose, concrete grammar is as follows: get 6.4g glucose and add in the 15.2g water, add 0.8g emulsion splitter (concentration 2 heavy %), and with flocculation agent (polyacrylamide, concentration 1 heavy %) mixes wiring solution-forming, give heat after 95 ℃, mix with the 160g slurry oil that is preheating to 100 ℃ in advance, click to mix 50 times with juice extractor, fall in test tube added electric field in the breakdown of emulsion instrument, leave standstill breakdown of emulsion and divide water, strength of electric field 2000v/cm, take out after 1 hour, extract lower layer of water out, get the slurry oil survey ash content that stirs.Test-results sees Table 6, finds out from table 6 data, and along with the increase of flocculation agent consumption, decreasing ratio increases, decreasing ratio when the flocculation agent dosage is 600ppm is the highest, reaches 93.2%, takes off back slurry oil ash content 0.0227%, when the flocculation agent dosage surpassed 600ppm, decreasing ratio no longer increased, and has a declining tendency.
The removal effect of the different flocculation agent dosages of table 6
Embodiment 5
The character of the slurry oil B that handles sees Table 4.Increase proportion with glucose, concrete grammar is as follows: get 9.1g glucose and add in the 21.6g water, add 0.8g emulsion splitter (FC9301, concentration 2 heavy %), and with 9.6g flocculation agent (polyacrylamide, concentration 1 heavy %) mix wiring solution-forming, flocculation agent dosage 600ppm, give heat after 95 ℃, mix, click with juice extractor and mix 50 times with the 160g slurry oil that is preheating to 100 ℃ in advance, place the pressurized vessel heating demulsification type, take out after 2 hours, extract lower layer of water out, get the slurry oil survey ash content that stirs.Test-results sees Table 7, and as seen from Table 7, under uniform temp, the removal effect of heating demulsification type is poor than added electric field, and along with temperature raises, decreasing ratio increases, and 125 ℃ decreasing ratio is near the effect of added electric field.
The removal effect of the different settling temperature of table 7
Embodiment 6
The character of the slurry oil B that handles sees Table 4.Increase proportion with ammonium citrate, adopt and once take off back oil, concrete grammar is as follows: get the 6.4g ammonium citrate and add in the 15.2g water, add 0.8g emulsion splitter (FC9301, concentration 2 heavy %), and mix wiring solution-forming with flocculation agent (polyacrylamide, the heavy % of concentration 1), be preheating to 95 ℃ after, once taking off back oil with the 160g that is preheating to 100 ℃ in advance mixes, click to mix 50 times with juice extractor, fall in test tube added electric field in the breakdown of emulsion instrument, leave standstill breakdown of emulsion and divide water, strength of electric field 2000v/cm, take out after 1 hour, extract lower layer of water out, get the slurry oil survey ash content that stirs.Test-results sees Table 8, find out from test-results, the ash content that once takes off back oil is between 0.04%-0.1%, the decreasing ratio that does not add flocculation agent is 61.5%, takes off the back putty and is divided into 0.0214%, along with the increase of flocculation agent dosage, decreasing ratio improves, ash content is 0.0443% before taking off, and during flocculation agent dosage 600ppm, the ash content that takes off the back slurry oil is 0.0057%.
The effect that table 8 secondary removes
Embodiment 7
The character of the slurry oil B that handles sees Table 4.Increase proportion with glucose, adopt reuse water, concrete grammar is as follows: the water 21.6g that fetches receipts, filter with the G3 sand core funnel, add 1.9g glucose, and with 0.8g emulsion splitter (concentration 2 heavy %), and with 9.6g flocculation agent (polyacrylamide, concentration 1 heavy %) mixes wiring solution-forming, after being preheating to 95 ℃, mix, click with juice extractor and mix 50 times with the 160g slurry oil that is preheating to 100 ℃ in advance, fall in the sub-test tube added electric field in the breakdown of emulsion instrument, leave standstill breakdown of emulsion and divide water, strength of electric field 2000v/cm took out after 1 hour, extract lower layer of water out, get the slurry oil survey ash content that stirs.Test-results sees Table 9, finds out from the result, adopts the decreasing ratio of reuse water slightly to descend, and is owing to also remaining in the reuse water medicament arranged, and adds to cause behind the medicament excessively, and decreasing ratio slightly descends, and need according to circumstances should reduce the amount of adding medicament.
Table 9 adopts the removal effect of reuse water
Comparative Examples:
The character of the slurry oil B that handles sees Table 4.Get the 100g slurry oil and place test tube, left standstill 24 hours in 95 ℃, get upper strata 50g and the 50g of lower floor slurry oil and survey ash content.Test-results sees Table 10, finds out from test-results, and the decreasing ratio of natural subsidence is lower, has only 18.4%.
The catalyst removal effect of table 10 standing sedimentation
Claims (7)
1. method that removes catalyst fines in the catalytically cracked oil, comprise: the water that will contain emulsion splitter and flocculation agent mixes with catalytically cracked oil, breakdown of emulsion, with enrichment the lower layer of water of catalyst fines tell, wherein the water yield is the heavy % of 5-30 of catalytically cracked oil weight, the emulsion splitter consumption is the 10-500ppm of the weight of slurry oil, and the consumption of flocculation agent is the 10-1000ppm of slurry oil weight.
2. in accordance with the method for claim 1, it is characterized in that water and catalytically cracked oil are preheating to 95-100 ℃ respectively, mix the back at 90-140 ℃ of following heating demulsification type, or under the 2000-5000v/cm electric field breakdown of emulsion.
3. in accordance with the method for claim 1, it is characterized in that the water yield is the heavy % of the 10-20 of catalytically cracked oil weight.
4. in accordance with the method for claim 1, it is characterized in that emulsion splitter is alkoxylated alkylphenol urea formaldehyde, polyvalent alcohol polyoxyethylene polyoxypropylene block copolymer, polyethylene polyamine polyoxyethylene polyoxypropylene block copolymer or its compound.
5. in accordance with the method for claim 1, it is characterized in that the emulsion splitter consumption is the 20-100ppm of the weight of slurry oil.
6. in accordance with the method for claim 1, it is characterized in that flocculation agent is polymerization silicate, poly-ferric chloride, polymerize aluminum chloride, Poly Dimethyl Diallyl Ammonium Chloride, polyacrylamide, sodium polyacrylate or acrylic acid-acrylamide copolymer.
7. in accordance with the method for claim 1, it is characterized in that the consumption of flocculation agent is the 200-1000ppm of slurry oil weight.
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| CN102304384A (en) * | 2011-08-12 | 2012-01-04 | 中国石油天然气股份有限公司 | Biological low-temperature dehydration demulsifier |
| US20140262936A1 (en) * | 2013-03-15 | 2014-09-18 | Sundance Services International Limited | System and method for cleaning and recovery of hydrocarbons |
| CN105523606B (en) * | 2015-12-30 | 2018-05-11 | 克拉玛依市三达新技术股份有限公司 | Compound reverse-phase emulsifier and preparation method thereof and application method |
| CN106318440B (en) * | 2016-09-21 | 2019-02-12 | 连云港爱华能源科技发展有限公司 | A kind of catalytic cracked oil pulp sedimentation agent and preparation method thereof, application |
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| CN109233902A (en) * | 2018-11-08 | 2019-01-18 | 黑龙江省能源环境研究院 | A kind of method of catalyst fines in removing catalytic slurry |
| CN109628142B (en) * | 2019-01-22 | 2022-10-18 | 中国石油大学(华东) | Method for efficiently removing solid particles in FCC (fluid catalytic cracking) oil slurry at low cost |
| CN111621322B (en) * | 2020-06-19 | 2022-02-22 | 金浦新材料股份有限公司 | Oil slurry settling agent and preparation method and application thereof |
| CN114540073A (en) * | 2020-11-20 | 2022-05-27 | 中国石油天然气股份有限公司 | Method for removing catalyst particles in catalytic cracking slurry oil |
| CN114181731B (en) * | 2021-12-07 | 2023-03-21 | 中海油天津化工研究设计院有限公司 | Micelle dispersion type oil slurry settling agent and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5681451A (en) * | 1996-01-31 | 1997-10-28 | Betzdearborn Inc. | Settling aids for solids in hydrocarbons |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5681451A (en) * | 1996-01-31 | 1997-10-28 | Betzdearborn Inc. | Settling aids for solids in hydrocarbons |
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