CN104020261A - Method for testing selectivity of catalyst - Google Patents
Method for testing selectivity of catalyst Download PDFInfo
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- CN104020261A CN104020261A CN201410276292.1A CN201410276292A CN104020261A CN 104020261 A CN104020261 A CN 104020261A CN 201410276292 A CN201410276292 A CN 201410276292A CN 104020261 A CN104020261 A CN 104020261A
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- catalyst
- sample
- selectivity
- unknown
- carburizing
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- 239000003054 catalyst Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000012360 testing method Methods 0.000 title claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 10
- 238000005255 carburizing Methods 0.000 claims description 23
- 150000001336 alkenes Chemical class 0.000 claims description 5
- 230000003197 catalytic effect Effects 0.000 claims description 5
- 230000009467 reduction Effects 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 238000011065 in-situ storage Methods 0.000 claims 1
- 238000011156 evaluation Methods 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract 2
- 229910052742 iron Inorganic materials 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 17
- 239000007789 gas Substances 0.000 description 12
- 239000000047 product Substances 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 230000006698 induction Effects 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZXKXJHAOUFHNAS-FVGYRXGTSA-N (S)-fenfluramine hydrochloride Chemical compound [Cl-].CC[NH2+][C@@H](C)CC1=CC=CC(C(F)(F)F)=C1 ZXKXJHAOUFHNAS-FVGYRXGTSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000013480 data collection Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 1
Abstract
The invention discloses a method for testing the selectivity of a catalyst. The aim of replacing the traditional catalyst evaluation method is achieved in a way of testing the carburization performance of a sample catalyst. The method comprises the three procedures of firstly, carrying out catalytic reaction evaluation on a known catalyst sample to obtain the selectivity S' of the known catalyst sample to low-carbon olefin; secondly, respectively testing the carburization performances of an unknown catalyst and a known catalyst to obtain the heights H and H' of CO consumption peaks formed by carburization curves within the temperature intervals of 365-455 DEG C; thirdly, calculating by using a relational expression: S/S'=H/H' to obtain the selectivity S of the unknown catalyst to low-carbon olefin. The method is particularly suitable for evaluating the selectivity of an iron catalyst to low-carbon olefin in a Fischer-Tropsch synthesis process.
Description
Technical field
The present invention relates to a kind of method of detecting catalyst, be specifically related to a kind of metallic catalyst method to C2 to C4 olefine selective in Fischer-Tropsch synthesis of testing.
Background technology
Fischer-Tropsch is synthetic is that to take CO and H2 be unstripped gas, under the effect of catalyzer, and the synthetic reaction with different carbon chain structure product.Dissimilar catalyzer has obvious performance difference in Fischer-Tropsch building-up process, this species diversity is mainly manifested in the selectivity of reaction product, pure Fe catalyzer for example, in its Fischer-Tropsch synthetic, mostly be saturated hydro carbons, and added K or Mn as auxiliary agent after, in catalytic reaction products, the content of unsaturated hydro carbons obviously improves.
Traditional fischer-tropsch synthetic catalyst test evaluation method is that a certain amount of catalyst sample is placed in reaction tube, first passing into H2 reduces catalyst sample at a certain temperature, then the synthetic gas of the different H2/ CO ratios as reaction raw materials is passed into reactor, under certain reaction conditions, catalyzed conversion effect through catalyzer, generate the product of different structure, these products are formed to content by instrument monitoring analyses such as chromatogram, mass spectrums, through data preparation, draw the reactivity worth result that comprises selectivity of this catalyst sample.Due to the existence of decomposition induction time, the catalytic performance data that obtain within induction period are not the true reflections of catalyst performance, and therefore traditional evaluation response time at least will be more than 10 hours, and the reaction result data of the sample obtaining are like this just substantially credible.This shows, be a process very consuming time by classic method evaluate catalysts.In order to improve the efficiency of evaluating catalyst process, the invention provides a kind of can the method for Fast Evaluation catalyzer to selectivity of light olefin, the method, is the carburizing performance quick obtaining sample selectivity of utilizing test sample.So-called carburizing performance is because metallics in catalyzer is different from the chemical action between CO molecule, and catalyst sample can, along with temperature variation, show different CO and consume trend in CO atmosphere.The time of carburizing test generally can not surpass 90 minutes, than traditional evaluation time of at least 10 hours, has greatly shortened.
Summary of the invention
The object of the present invention is to provide a kind of can detecting catalyst in Fischer-Tropsch synthesis to low-carbon alkene (namely ethene, propylene and butylene and isomeride thereof) method optionally, by comparing unknown catalyst sample and known catalysts in carburizing test, carburizing curve in 365 ℃ to 455 ℃ warm areas forms CO and consumes the high relation of peak-to-peak, obtains fast the selectivity of unknown catalyst sample to low-carbon alkene.
The method of a kind of detecting catalyst provided by the invention to selectivity of light olefin, basic step comprises three programs below, program one, carries out catalytic reaction evaluation to known catalysts sample, obtains its selectivity S ' to low-carbon alkene; Program two, carries out carburizing performance test to unknown catalyzer and known catalysts respectively, obtains peak height H and the H ' at the peak that in each comfortable 365 ℃ to 455 ℃ temperature ranges, carburizing curve forms; Program three, utilizes relational expression S/S '=H/H ', obtains the selectivity S of unknown catalyzer to low-carbon alkene.
Concrete, program one, be the process of catalytic reaction evaluation that known catalyst sample is carried out, concrete operations condition is as follows, takes the catalyzer of 0.1g to 10g, at 300 ℃ to 500 ℃, under pressure 0MPa to 5MPa, with H2 reduction 1 hour to 5 hours, then gas is switched to the synthetic gas of H2/CO=3, at pressure 2MPa to 6MPa, in the volume space velocity GHSV(unit interval, pass through the volume of the reactant of per volume of catalyst) 200hr
-1to 10000hr
-1, reaction at 200 ℃ to 500 ℃ of temperature of reaction, react 10 hours above after, the content of each component in employing gas chromatographic detection assay products, low-carbon alkene (alkene of C2 to C4) selectivity S ' (by weight percentage)=(∑ C
n =)/(∑ C
nh
2n+2+ ∑ C
nh
2n), n=2 here, 3,4.
Program two, is respectively unknown catalyzer and known catalysts to be carried out to carburizing performance test, obtains peak height H and the H ' at the peak that in each comfortable 365 ℃ to 455 ℃ temperature ranges, carburizing curve forms.The process of carburizing test is, 200 ℃ to 600 ℃, under 0 MPa to 5MPa, with H2 by sample preparation after 1 hour to 4 hours, in H2 atmosphere, be cooled to after room temperature,, by catalyst sample bed, flow control is at 1mLmin to switch to CO gas with inert gas dilution (CO account for cumulative volume 0.1% to 20%)
-1g
-1catalyzer is to 20mLmin
-1g
-1in range of catalysts, start to heat up to catalyst sample simultaneously, the speed heating up is 1 ℃/min to 20 ℃/min, with the detecting device that can detect online CO content, detect the consumption of CO under different temperatures, formation be take temperature as horizontal ordinate, the carburizing curve that the CO signal intensity that the instrument of take detects is ordinate, and the detecting device that detects online CO content can be thermal conductivity detector (TCD), mass detector, infrared detector.
Program three, S ', the H and H ' substitution relational expression the S/S '=H/H ' that in program one and program two, obtain, calculate the selectivity S of unknown catalyzer to low-carbon alkene.
Said process completes on same hardware platform, and this platform comprises, induction system, and reactive system, reaction product detects analytic system; In induction system, different media flows in different pipelines, controls the flow of gas with different mass-flow gas meters, with volume pump, controls and carry liquid; Reactive system comprises, the reaction member of loading catalyst sample and the unit that reaction institute energy requirement is provided, reaction member can be single pass, also can be multichannel, the manufacture material of reaction member can be metal, can be also quartzy, it can be Resistant heating that the energy supply form of the unit of reaction institute energy requirement is provided, Elema heating, can be also microwave energy supply, plasma energy supply; Reaction product detects analytic system and comprises detector system and the corresponding data collection analysis system that can detect online the product composition flowing out from reaction member, and detection system can be chromatographic detector, mass detector, infrared detector.
Accompanying drawing explanation
Fig. 1 is the carburizing curve of test known sample HA202Q.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further detailed.
The following examples are only for the present invention that explains in detail, and limit the scope of the invention never in any form.
Embodiment 1
First, evaluate known catalyst sample, it is a kind of commercially available synthetic ammonia catalyst HA202Q(Pingxiang City Parkson chemical filler company limited), take this catalyst sample of 1g, at 400 ℃, under 2.5MPa, with H2 reduction 3 hours, then gas is switched to the synthetic gas of H2/CO=3, at pressure 3MPa, volume space velocity GHSV=800hr
-1, reaction at 320 ℃ of temperature of reaction, while react 12 hours, the content of each component in employing gas chromatographic detection assay products, low-carbon alkene (alkene of C2 to C4) selectivity S '=45.3%
Then, be that HA202Q is carried out to carburizing performance test, take this sample of 1g, 400 ℃, under 2MPa, with H2 reductase 12 hour, in H2 atmosphere, be cooled to room temperature,, by catalyst sample bed, flow control is at 10mLmin then to switch to CO gas with inert gas dilution (CO account for cumulative volume 10%)
-1g
-1catalyzer, start to heat up to catalyst sample simultaneously, the speed heating up is 10 ℃/mi, with online mass detector (Omnistar 300), detect the CO content flowing out in reaction member, form as the carburizing curve of Fig. 1, the peak that carburizing curve forms in 365 ℃ to 455 ℃ temperature ranges is as the peak P in Fig. 1, peak maximum P to this on baseline WE between subpoint K the length of line segment PK be peak height H ', according to the data result of test, H '=4.0 * 10
-11ev.
Getting off, is that unknown catalyzer is carried out to carburizing performance test again, and test condition is the same (selecting the HTA206 ammonia synthesis catalyst of Liaoning Haitai development in science and technology company limited here as unknown catalyzer) with test during HA202Q.The carburizing curve that test obtains in 365 ℃ to 455 ℃ temperature ranges, form CO peak height H=4.3 * 10 that consume peak
-11ev.
Finally, according to relational expression S/S '=H/ H ', can obtain unknown catalyzer (HTA206) in Fischer-Tropsch synthesis to the selectivity S=of low-carbon alkene (H/H ') * S '=48.7%.
Claims (4)
1. detecting catalyst method optionally, it is characterized in that, by comparing the carburizing performance of the sample of unknown catalyzer and known catalytic performance, obtain the result of unknown catalyst selectivity (S), especially Fischer-Tropsch synthesizes the selectivity that in the catalytic process of producing alkene, carbon two is arrived the low-carbon alkene of carbon four.
2. a kind of detecting catalyst according to claim 1 method optionally, is characterized in that, the test process of carburizing performance is operating as,
The first step, carries out the reduction of H2 and processes to catalyst sample;
Second step, with the gas that contains CO, the sample in-situ of being processed by H2 reduction in the first step is carried out to Carburization Treatment, the online consumption that detects CO under different temperatures, forms and take temperature as horizontal ordinate simultaneously, the carburizing curve that the CO signal intensity that the instrument of take detects is ordinate.
3. a kind of detecting catalyst according to claim 1 method optionally, it is characterized in that, when the carburizing performance of comparing the sample of unknown catalyzer and known catalytic performance obtains unknown catalyst selectivity result, the peak height that the CO that both carburizing curves form of take consumes peak is comparison other, the peak height that unknown sample forms is (H), the peak height of known catalytic performance sample is (H '), between the selectivity of unknown catalyst sample (S) and known sample selectivity (S '), meets relational expression S/S '=H/H '.
4. a kind of detecting catalyst according to claim 3 method optionally, is characterized in that, what participate in comparison is the peak that in 365 ℃ to 455 ℃ temperature ranges, carburizing curve forms.
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| CN201410276292.1A CN104020261B (en) | 2014-06-19 | 2014-06-19 | A kind of detecting catalyst optionally method |
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| CN201410276292.1A CN104020261B (en) | 2014-06-19 | 2014-06-19 | A kind of detecting catalyst optionally method |
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| CN104020261B CN104020261B (en) | 2015-12-02 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770452A (en) * | 2017-01-26 | 2017-05-31 | 芜湖市纽泰知识产权信息咨询有限公司 | A kind of method that utilization thermal analysis system evaluates catalyst |
| CN106802262A (en) * | 2017-01-26 | 2017-06-06 | 芜湖市纽泰知识产权信息咨询有限公司 | A kind of method that utilization DTG tests catalyst performance |
| CN106841293A (en) * | 2017-01-26 | 2017-06-13 | 芜湖市纽泰知识产权信息咨询有限公司 | A kind of method that utilization difference quotient thermogravimetric evaluates catalyst |
| CN106841294A (en) * | 2017-01-26 | 2017-06-13 | 芜湖市纽泰知识产权信息咨询有限公司 | A kind of method that catalytic performance is evaluated in differential thermal analysis |
| CN110361499A (en) * | 2018-04-09 | 2019-10-22 | 国家能源投资集团有限责任公司 | The method of iron-base fischer-tropsch synthesis catalyst activity rating |
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| EP0128302A1 (en) * | 1983-05-16 | 1984-12-19 | Allied Corporation | Iron/silicon-based catalyst exhibiting high selectivity to C2-C6 alkenes in CO/H2 Fischer-Tropsch reactions |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770452A (en) * | 2017-01-26 | 2017-05-31 | 芜湖市纽泰知识产权信息咨询有限公司 | A kind of method that utilization thermal analysis system evaluates catalyst |
| CN106802262A (en) * | 2017-01-26 | 2017-06-06 | 芜湖市纽泰知识产权信息咨询有限公司 | A kind of method that utilization DTG tests catalyst performance |
| CN106841293A (en) * | 2017-01-26 | 2017-06-13 | 芜湖市纽泰知识产权信息咨询有限公司 | A kind of method that utilization difference quotient thermogravimetric evaluates catalyst |
| CN106841294A (en) * | 2017-01-26 | 2017-06-13 | 芜湖市纽泰知识产权信息咨询有限公司 | A kind of method that catalytic performance is evaluated in differential thermal analysis |
| CN106841293B (en) * | 2017-01-26 | 2019-05-28 | 王宏铭 | A method of catalyst is evaluated using difference quotient thermogravimetric |
| CN106770452B (en) * | 2017-01-26 | 2019-05-28 | 王宏铭 | A method of catalyst is evaluated using thermal analysis system |
| CN106802262B (en) * | 2017-01-26 | 2019-05-28 | 王宏铭 | A method of catalyst performance is tested using thermogravimetry |
| CN106841294B (en) * | 2017-01-26 | 2019-05-28 | 王宏铭 | A kind of method of differential thermal analysis evaluation catalytic performance |
| CN110361499A (en) * | 2018-04-09 | 2019-10-22 | 国家能源投资集团有限责任公司 | The method of iron-base fischer-tropsch synthesis catalyst activity rating |
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