CN104931381A - Method for detecting content of catalyst of catalytic slurry oil - Google Patents
Method for detecting content of catalyst of catalytic slurry oil Download PDFInfo
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- CN104931381A CN104931381A CN201510351067.4A CN201510351067A CN104931381A CN 104931381 A CN104931381 A CN 104931381A CN 201510351067 A CN201510351067 A CN 201510351067A CN 104931381 A CN104931381 A CN 104931381A
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Abstract
A method for detecting content of a catalyst of catalytic slurry oil comprises the following steps of measuring density of the slurry oil; diluting the slurry oil by using oily diluents until the density of the slurry oil is smaller than and equal to 1g/cm(3) when the density of the slurry oil is greater than 1g/cm(3); carrying out the following steps if the density of the slurry oil is smaller than or equal to 1g/cm(3): taking a certain amount of the slurry oil which is subjected to water bath preheating and is stirred sufficiently in a centrifuge tube, adding water-based diluting and demulsifying agents in the centrifuge tube, sufficiently mixing the slurry oil and the water-based diluting and demulsifying agents, treating the centrifuge tube in an ultrasonic generator and performing centrifugal sedimentation on the centrifuge tube in a centrifugal machine; removing a liquid portion; moving deposited solid catalyst on weighed filter paper; washing the deposited solid catalyst by using hot deionized water; and drying the filter paper and the catalyst until the weight of the filter paper and the weight of the catalyst are constant so as to obtain the solid content of the catalyst. The method is easy and quick to operate and accurate in measurement result.
Description
Technical field
The present invention relates to a kind of catalytic slurry analyzing detecting method, particularly a kind of catalytic slurry catalyst content detection method.
Background technology
Current China catalytic slurry total production is about 7-8Mt/a, catalytic slurry H/C is about 1.1-1.3, saturated point, fragrance point and gum asphalt be about 30%, 60% and 8% respectively, can be used for the acicular petroleum coke of deep processing production high-quality, carbon black and rubber softening wet goods, but due to catalyst fines content in slurry oil higher (some slurry oil dust content is up to about 6 grams per liters), tired reasonable development application of scratching catalytic cracked oil pulp.
The main method measuring solid content of oil slurry has: the Standard test method, carbonization calcination method etc. of total residue content in centrifuge method, petroleum products Ash determination method, mensuration residual oil.All there is deficiency to a certain degree in these methods, centrifuge method is to the slurry oil of high bituminous matter, gum level, and precision is not high; Carbonization calcination method measurement result is subject to again inorganic salts interference; It is comparatively cumbersome or require the problems such as high to instrument and examination material then to there is operation in petroleum products Ash determination method and the Standard test method measuring total residue content in residual oil.
Summary of the invention
The object of the invention is to the deficiency existed for current catalytic cracked oil pulp solids content analysis test method, provide a kind of new catalytic slurry oil admittedly containing analytical approach, the method is simple to operate, quick, measurement result is accurate.
Object of the present invention can be achieved by the following technical measures:
A kind of catalytic slurry catalyst content detection method, first measures the density of slurry oil, as the density≤1g/cm of slurry oil
3in time, carries out in the steps below, and works as the density >1g/cm of slurry oil
3shi Xianyong oiliness thinning agent is diluted to the density≤1g/cm of slurry oil
3, and then carry out in the steps below:
Get a certain amount of this slurry oil after water-bath preheating and abundant stirring in centrifuge tube, add water-based dilution-emulsion breaker wherein, make it fully mixed, centrifuge tube is put into ultrasonic generator and processes, then put into hydro-extractor centrifugal settling; Remove liquid part, on the filter paper that the solid catalyst dislocation of precipitation has been weighed, wash with the deionized water of heat, filter paper and catalyzer are dried to constant weight, catalyzer solid content can be calculated.
In above-mentioned, slurry oil is preheated to 40-50 DEG C through water-bath.
In above-mentioned, the mixed aqueous solution that the quality such as this water-based dilution-emulsion breaker is hexadecyltrimethylammonium chloride, two or more compound in OTAC, dodecyl benzyl dimethyl ammonium chloride, polyvinylpyrrolidone, polyglycol are mixed with, the mass concentration of this mixed aqueous solution is 50-500 μ g/g.
In above-mentioned, the consumption of water-based dilution-emulsion breaker is 1-2.5 times of slurry oil quality.
In above-mentioned, ultrasonic process is at temperature 60 C, power 40-400W, frequency 20-80KH
zcondition under process 2-15min.
In above-mentioned, centrifugal rotational speed 2000-5000r/min, centrifugation time 2-8min during centrifugal settling process in hydro-extractor.
In above-mentioned, with 50-80 DEG C of deionized water washing, the number of times of washing is 2-3 time.
In above-mentioned, oiliness thinning agent used is the molar mixtures such as any two kinds in normal hexane, sherwood oil, dimethylbenzene.
The present invention is simple to operate, quick, measurement result is accurate.
Embodiment
Embodiment one:
Take the catalytic slurry sample of 18.5890 grams, slurry oil density 0.9381g/cm
3being preheated to 45 DEG C through water-bath is placed in centrifuge tube with fully stirring, and adds the water-based dilution-emulsion breaker of 29.6320 grams wherein, fully mixes, centrifuge tube is put into ultrasonic field and carries out ultrasonic process, the condition of ultrasonic process is temperature 60 C, power 300W, frequency 80KH
zlower process 5min.Centrifugal settling again, rotating speed 2500r/min, time 4.5min.Remove liquid part, be on the filter paper of 1.280 grams, wash 2 times with 30mL, 80 DEG C of deionized waters by the solid catalyst dislocation quality of precipitation gained, drying filter paper and catalyzer to constant weight is 1.2926 grams, and calculating catalyzer solid content is 677.8 μ g/g.
Institute's use dilution-emulsion breaker is the mass mixing aqueous solution such as hexadecyltrimethylammonium chloride, dodecyl benzyl dimethyl ammonium chloride, polyvinylpyrrolidone, and the mass concentration of mixed aqueous solution is 97.20 μ g/g.
Embodiment two:
Take the catalytic slurry sample of 26.3870 grams, slurry oil density 0.9560g/cm
3being preheated to 45 DEG C through water-bath is placed in centrifuge tube with fully stirring, and adds the water-based dilution-emulsion breaker of 40.4550 grams wherein, fully mixes, centrifuge tube is put into ultrasonic field and carries out ultrasonic process, the condition of ultrasonic process is at temperature 60 C, power 150W, frequency 30KH
zlower process 8min.Centrifugal settling again, rotating speed 3000r/min, time 5min.Remove liquid part, be on the filter paper of 1.280 grams, wash 2 times with 40mL, 80 DEG C of deionized waters by the solid catalyst dislocation quality of precipitation gained, drying filter paper and catalyzer to constant weight is 1.3195 grams, and calculating catalyzer solid content is 1496.9 μ g/g.
Institute's use dilution-emulsion breaker is the mass mixing aqueous solution such as hexadecyltrimethylammonium chloride, OTAC, polyglycol, and the mass concentration of mixed aqueous solution is 120.20 μ g/g.
Embodiment three:
Take the catalytic slurry sample of 20.5610 grams, slurry oil density 0.9560g/cm
3being preheated to 45 DEG C through water-bath is placed in centrifuge tube with fully stirring, and adds the water-based dilution-emulsion breaker of 35.2650 grams wherein, fully mixes, centrifuge tube is put into ultrasonic field and carries out ultrasonic process, the condition of ultrasonic process is at temperature 60 C, power 80W, frequency 40KH
zlower process 10min.Centrifugal settling again, rotating speed 3500r/min, time 4min.Remove liquid part, be on the filter paper of 1.280 grams, wash 2 times with 40mL, 80 DEG C of deionized waters by the solid catalyst dislocation quality of precipitation gained, drying filter paper and catalyzer to constant weight is 1.3110 grams, and calculating catalyzer solid content is 1507.7 μ g/g.
Institute's use dilution-emulsion breaker is the mass mixing aqueous solution such as hexadecyltrimethylammonium chloride, dodecyl benzyl dimethyl ammonium chloride, polyvinylpyrrolidone, and the mass concentration of mixed aqueous solution is 97.20 μ g/g.
Embodiment four:
Take the catalytic slurry sample of 21.8620 grams, slurry oil density 1.0963g/cm
3, add wherein oiliness thinning agent sherwood oil, dimethylbenzene etc. mass mixing thing, the density being diluted to slurry oil is 0.9660g/cm
3, be preheated to 45 DEG C through water-bath and be placed in centrifuge tube with fully stirring, then add the aqueous diluent of 30.2310 grams in sample, fully mix, centrifuge tube is put into ultrasonic field process, the condition of ultrasonic process is at temperature 60 C, power 100W, frequency 60KH
zlower process 10min.Centrifugal settling again, rotating speed 3000r/min, time 6min.Remove liquid part, be on the filter paper of 1.280 grams, wash 2 times with 40mL, 80 DEG C of deionized waters by the solid catalyst dislocation quality of precipitation gained, drying filter paper and catalyzer to constant weight is 1.3036 grams, and calculating catalyzer solid content is 1079.5 μ g/g.Carbon calcination method records this slurry oil admittedly containing being 1083.10 μ g/g.Two kinds of method errors 0.33%.
Institute's use dilution-emulsion breaker is the mass mixing aqueous solution such as hexadecyltrimethylammonium chloride, OTAC, polyglycol, and the mass concentration of mixed aqueous solution is 120.20 μ g/g.
Claims (8)
1. a catalytic slurry catalyst content detection method, is characterized in that, first measures the density of slurry oil, as the density≤1g/cm of slurry oil
3in time, carries out in the steps below, and works as the density >1g/cm of slurry oil
3shi Xianyong oiliness thinning agent is diluted to the density≤1g/cm of slurry oil
3, and then carry out in the steps below:
Get a certain amount of this slurry oil after water-bath preheating and abundant stirring in centrifuge tube, add water-based dilution-emulsion breaker wherein, make it fully mixed, centrifuge tube is put into ultrasonic generator and processes, then put into hydro-extractor centrifugal settling; Remove liquid part, on the filter paper that the solid catalyst dislocation of precipitation has been weighed, wash with the deionized water of heat, filter paper and catalyzer are dried to constant weight, catalyzer solid content can be calculated.
2. a kind of catalytic slurry catalyst content detection method according to claim 1, it is characterized in that, slurry oil is preheated to 40-50 DEG C through water-bath.
3. a kind of catalytic slurry catalyst content detection method according to claim 1, it is characterized in that, the mixed aqueous solution that the quality such as this water-based dilution-emulsion breaker is hexadecyltrimethylammonium chloride, two or more compound in OTAC, dodecyl benzyl dimethyl ammonium chloride, polyvinylpyrrolidone, polyglycol are mixed with, the mass concentration of this mixed aqueous solution is 50-500 μ g/g.
4. a kind of catalytic slurry catalyst content detection method according to claim 3, is characterized in that, the consumption of water-based dilution-emulsion breaker is 1-2.5 times of slurry oil quality.
5. a kind of catalytic slurry catalyst content detection method according to claim 1, it is characterized in that, ultrasonic process is at temperature 60 C, power 40-400W, frequency 20-80KH
zcondition under process 2-15min.
6. a kind of catalytic slurry according to claim 1 is admittedly containing detection method, it is characterized in that, centrifugal rotational speed 2000-5000r/min, centrifugation time 2-8min during centrifugal settling process in hydro-extractor.
7. a kind of catalytic slurry catalyst content detection method according to claim 1, is characterized in that, with 50-80 DEG C of deionized water washing, the number of times of washing is 2-3 time.
8. a kind of catalytic slurry catalyst content detection method according to claim 1, is characterized in that, oiliness thinning agent used is the molar mixtures such as any two kinds in normal hexane, sherwood oil, dimethylbenzene.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105842108A (en) * | 2016-03-22 | 2016-08-10 | 中国石油大学(华东) | Method for determination of solid content of catalytic cracking oil slurry |
| CN106929096A (en) * | 2017-05-05 | 2017-07-07 | 黑龙江省能源环境研究院 | A kind of catalytic cracked oil pulp pretreatment system and the method pre-processed using the system |
| CN107703020A (en) * | 2017-10-18 | 2018-02-16 | 中石化炼化工程（集团）股份有限公司 | A kind of method for determining wax tailings solid content |
| 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 |
| CN109355096A (en) * | 2018-12-15 | 2019-02-19 | 陕西延长石油（集团）有限责任公司 | A kind of method that coal-derived oils are separated by solid-liquid separation |
| CN113804579A (en) * | 2020-06-16 | 2021-12-17 | 中国石油天然气股份有限公司 | Sample rack for determining catalyst content in oil slurry by ash method and test method |
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| CN101665717A (en) * | 2009-10-14 | 2010-03-10 | 中国石油化工股份有限公司 | Method for removing remnant solid particles in catalytic cracking slurry oil by ultrasonic enhancement |
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| US4686048A (en) * | 1981-12-23 | 1987-08-11 | Exxon Research & Engineering Co. | Process for treating cat cracker bottoms sludge |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105842108A (en) * | 2016-03-22 | 2016-08-10 | 中国石油大学(华东) | Method for determination of solid content of catalytic cracking oil slurry |
| CN106929096A (en) * | 2017-05-05 | 2017-07-07 | 黑龙江省能源环境研究院 | A kind of catalytic cracked oil pulp pretreatment system and the method pre-processed using the system |
| CN106929096B (en) * | 2017-05-05 | 2019-03-26 | 黑龙江省能源环境研究院 | A kind of catalytic cracked oil pulp pretreatment system and the system is utilized to carry out pretreated method |
| CN107703020A (en) * | 2017-10-18 | 2018-02-16 | 中石化炼化工程（集团）股份有限公司 | A kind of method for determining wax tailings solid content |
| 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 |
| CN109355096A (en) * | 2018-12-15 | 2019-02-19 | 陕西延长石油（集团）有限责任公司 | A kind of method that coal-derived oils are separated by solid-liquid separation |
| CN113804579A (en) * | 2020-06-16 | 2021-12-17 | 中国石油天然气股份有限公司 | Sample rack for determining catalyst content in oil slurry by ash method and test method |
| CN113804579B (en) * | 2020-06-16 | 2023-08-22 | 中国石油天然气股份有限公司 | Sample rack for measuring catalyst content in slurry oil by ash separation method and testing method |
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