CN1043567A - Micro anti-active index rapid assay methods and instrument - Google Patents
Micro anti-active index rapid assay methods and instrument Download PDFInfo
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- CN1043567A CN1043567A CN 88109728 CN88109728A CN1043567A CN 1043567 A CN1043567 A CN 1043567A CN 88109728 CN88109728 CN 88109728 CN 88109728 A CN88109728 A CN 88109728A CN 1043567 A CN1043567 A CN 1043567A
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Abstract
A kind ofly be applied in fast measuring instrument and the method that mensuration is the molecular sieve cracking catalyst micro anti-active index of raw material with the wax oil, it is characterized in that the raw material that uses is the monomer hydro carbons, simplified operation, equipment is little, finding speed is fast; Improve work efficiency 6-7 doubly than conventional ASTM3907-80 instrument and method.People's single analyses can be finished in 20-30 minute.Instrument of the present invention and method accurately and reliably, test result is compared with conventional method, error<± 2, degree of confidence can reach 95%, relative standard deviation<2%.This instrument also can calculate dynamic activity and the print result of equilibrium catalyst UOP except that can directly printing little index MA alive.
Description
The present invention relates to used a kind of method and the instrument of estimating the micro anti-active index (MA) of molecular sieve cracking catalyst of petroleum refining industry
Technical background:
Conventional molecular sieve cracking catalyst micro anti-active index is measured used method and apparatus, the main ASTM-D3907-80 method that adopts the U.S., the used equipment of this method comprises: the covering devices such as gas chromatographicanalyzer of water vapour pretreatment unit (water vapour deactivation), catalyst cracker and product.Wherein micro anti-active index is that the light diesel fuel with standard is a raw material, uses the molecular sieve cracking catalyst after the water vapour deactivation, reacts under 482 ℃, calculates the total conversion of its diesel oil weight, and this diesel oil total conversion is promptly as micro anti-active index.China is domestic also once to have some to ASTM method in addition improved assay method and instrument.But existing little activity determination method commonly used, exist all that equipment is huge, finding speed is slow, complex operation, time-consuming shortcoming, only cracking reaction and little index alive are tested this two work, need 1-2 people at least, spend 4-6 hour and just can finish, can not satisfy the needs of production control.
The purpose of invention: for solving aforesaid problem first purpose of the present invention is to improve finding speed, and concrete means are to utilize new method to simplify the operation, and simplified apparatus reduces manpower.
Second purpose of the present invention is the huge problem of solution equipment, use that a kind of volume is little, in light weight, simple in structure, cost is low, power consumption less, few, the easy to operate instrument of amount of samples.
The general introduction of invention:
The present invention is as the improved a kind of method of catalytic cracking reaction and MA mensuration aspect of ASTM-D3907-80, and its feature at first is employed raw material difference, thereby has produced a series of effect of the present invention.
1) method
Raw material used in the present invention is not the light diesel fuel of standard, but adopts the detailed hydrocarbon of CnHm, and n is 8-10; M is 10-14, and best raw material is C
9H
12Aromatic hydrocarbons.
Raw material enters reactor with carrier gas and carries out cracking reaction, and reaction product and not by the raw material of cracking is separated and identified by monitor in chromatographic column, by chromatographic data processor record spectrogram and calculate and print result.
The experiment condition of this method:
Temperature of reaction: 280-500 ℃
Post constant temperature oven: 100-180 ℃
Hot-wire temperature: 100-180 ℃
Carrier gas N
2Or H
2Or He
Flow velocity: 25-40ml/min
Range 1-16mV/ full scale
Catalytic amount 0.05-0.2g
Feedstock oil 2-10 μ l
2) instrument
See Fig. 1.Comprise microreactor (1), chromatograph (2), temperature controller (3) and chromatographic data processor (4) that the present invention assembles.The chromatographic data result is by chromatographic data processor formula of the present invention:
Y=aX+b
Handled and print result.
In the formula: Y represents the micro anti-active index MA(% of catalyzer)
X represents the production rate (%, computer-internal data) of reactant
a=0.2-0.9
b=10-60
The computer programme flow diagram of micro anti-active index is seen Fig. 2 in the chromatographic data processor software.
The chromatographic data processor of instrument of the present invention can also be according to the dynamic activity of conventional formula calculated equilibrium catalyzer UOP, when input coke productive rate, with regard to the printable result of calculation that goes out the UOP dynamic activity.
Embodiment:
Example 1. takes by weighing FCC apparatus poising agent 1#0.05 ± 0.001g, temperature of reaction: 300 ℃, feedstock oil 5 microlitres, coke productive rate: 3.5%(is heavy), print result then:
Micro anti-active index: 57.3(%) (conventional method records: 58.0)
UOP dynamic activity: 0.38
Example 2. catalytic cracking fixed bed device poising agent 2#0.1 ± 0.01g, temperature of reaction: 400 ℃, feedstock oil 10 microlitres, then print result:
Micro anti-active index (MA): 59.5(%) (conventional method records: 59.4)
Example 3. took by weighing fresh molecular sieve cracking catalyst 1#(water vapour deactivation 4 hours) 0.2 ± 0.01g, temperature of reaction: 450 ℃, raw material oil mass 2 microlitres, print result:
Micro anti-active index (MA): 80.0(%) (conventional method records: 79.9)
The effect of invention:
First purpose of the present invention reaches, and makes single analyses Zhi need 1 people, just can finish mensuration work (not comprising 30 minutes equilibration time of instrument) in Yong 20-30 minute. Finding speed is accelerated greatly, and comparable conventional method improves work efficiency 6-7 doubly. Process does not need compressing tablet to process, thereby has simplified operation.
Second purpose of the present invention also reaches, and instrument volume ratio conventional method is little a lot. Instrument of the present invention can also calculate the UOP dynamic activity.
The scope of application of the inventive method and instrument is that the Zhi little alive of material counts Zai 40%-80%, the fresh molecular sieve Cracking catalyst after the water vapour deactivation and the mensuration of balance Cracking catalyst take wax oil as Yuan. Test result Zhun is really reliable, sees Table 1, compare Yu conventional method, and error<± 2, confidence level can reach 95%, and relative standard deviation<2% all meets the demands.
Table 1 precision of method and error
Zhu: t2,n-1=t
0.05,6α=2.45
Claims (5)
1, a kind of method of estimating the micro anti-active index (MA) of molecular sieve cracking catalyst and equilibrium catalyst, the Qi Te emblem is that the employed raw material of evaluation MA is not the light diesel fuel of employing standard, but employing detailed hydrocarbon, under given conditions, pass through reactor (1), chromatograph (2), chromatographic data processor (4) successively by Fig. 1, print computer result MA.
The condition of reaction is as follows:
Temperature of reaction: 280--500 ℃, (by temperature controller (3) control)
Post constant temperature oven: 100--180 ℃
Hot-wire temperature: 100--180 ℃
Carrier gas: N
2, or H
2, or He
Flow velocity: 25--40ml/min
Catalytic amount 0.05--0.28
Feedstock oil 2--10 μ l
Range: 1--16mv/ full scale.
2, by the described method of claim 1, its characteristic is the detailed hydrocarbon that raw material adopts CnHm, and n is 8-10, and m is 10-14,
3, by claim 1,2 described methods, its characteristic is that best raw material is C
9H
12Aromatic hydrocarbons.
4, a kind of instrument that is used for fast measuring micro anti-active index MA, comprise the reactor shown in Fig. 1 (1), chromatograph (2), temperature controller (3), chromatographic data processor (4), its characteristic is the software that contains the processing chromatographic data of Y=aX+b in the chromatographic data processor, in the formula: Y is the index MA little alive (%) of catalyzer, X is the production rate (%) of reactant, a:0.2-0.9 b:10-60 and the mechanism of directly printing MA result of calculation.
5, by the described instrument of claim 4, its characteristic is a computer programme flow diagram of representing little index MA alive of software Y=aX+b in the chromatographic data processor with Fig. 2.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN 88109728 CN1017934B (en) | 1988-12-19 | 1988-12-19 | Rapid measuring method and apparatus for micro anti-active index |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 88109728 CN1017934B (en) | 1988-12-19 | 1988-12-19 | Rapid measuring method and apparatus for micro anti-active index |
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CN1043567A true CN1043567A (en) | 1990-07-04 |
CN1017934B CN1017934B (en) | 1992-08-19 |
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CN 88109728 Expired CN1017934B (en) | 1988-12-19 | 1988-12-19 | Rapid measuring method and apparatus for micro anti-active index |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103575859A (en) * | 2013-10-14 | 2014-02-12 | 青岛惠城石化科技有限公司 | Method for rapidly representing activity of catalytic cracking catalyst |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1093107C (en) * | 1999-05-10 | 2002-10-23 | 复旦大学 | Gas-phase selective adsorption process for separating mixed dichlorobenzene |
-
1988
- 1988-12-19 CN CN 88109728 patent/CN1017934B/en not_active Expired
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103575859A (en) * | 2013-10-14 | 2014-02-12 | 青岛惠城石化科技有限公司 | Method for rapidly representing activity of catalytic cracking catalyst |
CN103575859B (en) * | 2013-10-14 | 2015-04-29 | 青岛惠城石化科技有限公司 | Method for rapidly representing activity of catalytic cracking catalyst |
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