CN111912939A - Evaluation device and evaluation method for efficiently evaluating performance of olefin purifier - Google Patents
Evaluation device and evaluation method for efficiently evaluating performance of olefin purifier Download PDFInfo
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- CN111912939A CN111912939A CN202010749838.6A CN202010749838A CN111912939A CN 111912939 A CN111912939 A CN 111912939A CN 202010749838 A CN202010749838 A CN 202010749838A CN 111912939 A CN111912939 A CN 111912939A
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- 150000001336 alkenes Chemical class 0.000 title claims abstract description 170
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 title claims abstract description 169
- 238000011156 evaluation Methods 0.000 title claims abstract description 64
- 238000000746 purification Methods 0.000 claims abstract description 193
- 239000012535 impurity Substances 0.000 claims abstract description 70
- 239000002994 raw material Substances 0.000 claims abstract description 67
- 239000012629 purifying agent Substances 0.000 claims abstract description 66
- 238000012360 testing method Methods 0.000 claims abstract description 65
- 238000003860 storage Methods 0.000 claims abstract description 22
- 238000011049 filling Methods 0.000 claims abstract description 20
- 239000007789 gas Substances 0.000 claims description 112
- 239000003795 chemical substances by application Substances 0.000 claims description 53
- 239000000463 material Substances 0.000 claims description 43
- 238000006243 chemical reaction Methods 0.000 claims description 34
- 238000007789 sealing Methods 0.000 claims description 29
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 28
- 229910052802 copper Inorganic materials 0.000 claims description 28
- 239000010949 copper Substances 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 20
- 239000003054 catalyst Substances 0.000 claims description 16
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 15
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 14
- 230000003009 desulfurizing effect Effects 0.000 claims description 14
- 239000007791 liquid phase Substances 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000012024 dehydrating agents Substances 0.000 claims description 12
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 12
- 238000006116 polymerization reaction Methods 0.000 claims description 12
- 230000004913 activation Effects 0.000 claims description 11
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 230000007062 hydrolysis Effects 0.000 claims description 6
- 238000006460 hydrolysis reaction Methods 0.000 claims description 6
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 6
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- 238000003825 pressing Methods 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
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- 239000012752 auxiliary agent Substances 0.000 claims description 5
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- 230000000007 visual effect Effects 0.000 claims description 5
- 239000011787 zinc oxide Substances 0.000 claims description 5
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- 239000011572 manganese Substances 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 239000013014 purified material Substances 0.000 claims description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 3
- 239000005751 Copper oxide Substances 0.000 claims description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 3
- 229910052785 arsenic Inorganic materials 0.000 claims description 3
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 3
- 229910000431 copper oxide Inorganic materials 0.000 claims description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 3
- 229910000464 lead oxide Inorganic materials 0.000 claims description 3
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims description 3
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 2
- 230000006324 decarbonylation Effects 0.000 claims description 2
- 238000006606 decarbonylation reaction Methods 0.000 claims description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 239000002516 radical scavenger Substances 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 5
- 238000012854 evaluation process Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 51
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 50
- 230000008569 process Effects 0.000 description 11
- 239000002912 waste gas Substances 0.000 description 11
- JJWKPURADFRFRB-UHFFFAOYSA-N carbonyl sulfide Chemical compound O=C=S JJWKPURADFRFRB-UHFFFAOYSA-N 0.000 description 8
- -1 polyethylene Polymers 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 6
- 239000004743 Polypropylene Substances 0.000 description 5
- 239000002585 base Substances 0.000 description 5
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- 238000005070 sampling Methods 0.000 description 5
- 238000007599 discharging Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000010926 purge Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005262 decarbonization Methods 0.000 description 2
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- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
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- 238000002156 mixing Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
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- 238000002360 preparation method Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000003440 toxic substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 150000001345 alkine derivatives Chemical class 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920001748 polybutylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000002685 polymerization catalyst Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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- 230000000087 stabilizing effect Effects 0.000 description 1
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- 239000002699 waste material Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
-
- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05B—CONTROL OR REGULATING SYSTEMS IN GENERAL; FUNCTIONAL ELEMENTS OF SUCH SYSTEMS; MONITORING OR TESTING ARRANGEMENTS FOR SUCH SYSTEMS OR ELEMENTS
- G05B19/00—Programme-control systems
- G05B19/02—Programme-control systems electric
- G05B19/04—Programme control other than numerical control, i.e. in sequence controllers or logic controllers
- G05B19/05—Programmable logic controllers, e.g. simulating logic interconnections of signals according to ladder diagrams or function charts
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- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Food Science & Technology (AREA)
- Biochemistry (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Automation & Control Theory (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to an evaluation device and an evaluation method for efficiently evaluating the performance of an olefin purifying agent, wherein the evaluation device comprises an olefin raw material system, a pretreatment system, a purification test system, an impurity analysis system, an olefin storage system and a control system, the purification test system comprises a plurality of purification reactors which are sequentially connected in series and are used for filling olefin purifying agents with the same or different functions, and a connecting pipe communicated with the impurity analysis system is arranged between every two adjacent purification reactors. The evaluation method comprises the following steps: and respectively filling olefin purifying agents with the same or different functions into the purifying reactors, starting the device, and evaluating the olefin purifying agents. Compared with the prior art, the invention forms an olefin purification device platform capable of comprehensively evaluating the effects of various purifiers, the evaluation process fully simulates the industrial application conditions including the olefin raw material condition, the full particles of the purifiers, the pretreatment condition, the purification working condition and the like, and one or more types of purifiers can be flexibly selected to carry out performance evaluation.
Description
Technical Field
The invention belongs to the technical field of olefin purification treatment, and relates to an evaluation device and an evaluation method for efficiently evaluating normal-temperature olefin purification performance of various olefin purifiers.
Background
Polyolefins (e.g., polyethylene, polypropylene, polybutylene, etc.) are widely used in various industries, but olefins need to be purified to be used as petrochemical raw materials. The purpose of refining is to remove various contaminants that cause process flow problems (reduced catalyst yield, reduced polymer yield, corrosion of equipment, etc.) and affect the quality of the final product (polymer coloration, etc.).
For example, the existing literature and industrial practice show that the existence of trace impurities in propylene is one of the main factors influencing the polymerization reaction and the product performance, and as the propylene polymerization catalyst is continuously updated, the requirements of the new generation of high-efficiency catalyst on the purity and the impurity content of the raw material propylene are more and more strict.
On the other hand, from the national conditions of China, the raw material source of polypropylene is generally propylene separated from refinery gas (mainly heavy oil fluidized catalytic cracking). Refinery gas has low cost and rich resources, and only has high impurity content, and a series of processing and refining treatment is required. For the harmful impurities, the main hydrocarbon impurities (such as ethane, ethylene, propane, alkyne and dialkene) can be removed by a gas separation and rectification device, but S (especially COS), CO and H in propylene2O、O2The content of impurities such As As and the like must be purified and removed to meet the requirement of polymerization grade propylene. At present, refinery gas is adopted to separate propylene into liquidThe apparatus for bulk phase polymerization generally has the following purification process: the liquid phase propylene material after gasification and rectification passes through a soda-fixing tower, a (COS) hydrolysis tower and a (H) reaction tower2S) a desulfurizing tower, an alkali fixation tower, a molecular sieve drying tower, an arsenic removal tower, a molecular sieve drying tower, a carbon monoxide removal tower, a deoxygenation tower and finally enters a propylene storage tank.
The most key in the purification treatment process is to load various cheap and easily-obtained catalysts for adsorption or reaction purification. Development research and industrial application for more than twenty years show that various domestic purification catalysts can meet the requirements of domestic large, medium and small polypropylene manufacturers on raw materials, and are continuously promoted to be new. Based on the above, how to effectively and truly evaluate the performance of various adsorption purification catalysts so as to timely master the performance change and influence factors of the purifying agent is a problem of close attention of catalyst manufacturers and catalyst purchasing manufacturers. Patent No. CN201510090087.0 and utility model No. CN201821589073.9 both describe a propylene purification system and a propylene purification method in detail, but neither of them mention a critical evaluation method and have not been used industrially. The invention patent with the patent number of CN200810113358.X introduces a normal temperature propylene refining process and various purifiers used in the process in detail, but does not refer to a key evaluation device and an evaluation process.
At present, when the performance of a certain purifying catalyst is evaluated in a laboratory, a fixed bed reactor filled with a particle size purifying agent is mostly selected, and the reactor is simple and stable to operate and small in test quantity, so that the reaction/adsorption mechanism can be deeply researched, but the particle size purifying agent can not effectively obtain and monitor key data required by some industrial applications, such as pressure drop of a purifying system under a working condition, the performance of a full particle purifying agent and other parameters, because factors such as internal and external diffusion, small filling quantity and the like are eliminated. Meanwhile, the types and the contents of toxic substances contained in different olefin raw materials in the industry are different, the existing olefin purification device has the problem of poor pertinence, and the device only for evaluating the purification performance of a single impurity not only wastes equipment, but also seriously interferes the evaluation result of the purification performance due to the existence of other impurities, thereby influencing the accuracy of the measurement result. The invention patent with the patent number of 201810582892.9 and the utility model patent with the patent number of 201920158505.9 respectively introduce an evaluation device or a process for deoxidizing or dearsenifying compounds in propylene; the utility model with 201920076302.5 discloses two desulfurization catalyst evaluation devices, but is not suitable for evaluating other purifiers.
In summary, the device for evaluating the comprehensive performance of various olefin purifiers in China is still blank at present, so that the device for evaluating the performance of the normal-temperature olefin purifiers has higher practical value and economic value.
Disclosure of Invention
The invention aims to provide an evaluation device and an evaluation method for efficiently evaluating the performance of an olefin purifying agent, wherein the evaluation device can simulate the purifying capacity of various purifying agents on multi-component impurities in an olefin raw material under a working condition, and has the advantages of capability of evaluating various olefin purifying agents, better applicability, closer working condition conditions and the like.
The purpose of the invention can be realized by the following technical scheme:
an evaluation device for efficiently evaluating the performance of an olefin purifier comprises an olefin raw material system, a pretreatment system, a purification test system, an impurity analysis system, an olefin storage system and a control system, the purification test system comprises a plurality of purification reactors which are sequentially connected in series and are used for filling olefin purifiers with the same or different functions, a connecting pipe communicated with the impurity analysis system is arranged between every two adjacent purification reactors, the feed end of the purification test system is respectively communicated with the olefin raw material system, the pretreatment system and the impurity analysis system, the discharge end of the purification test system is respectively communicated with the impurity analysis system and the olefin storage system, the control system is respectively and electrically connected with the olefin raw material system, the pretreatment system, the purification test system, the impurity analysis system and the olefin storage system.
Furthermore, the olefin raw material system comprises an olefin raw material tank and a high-pressure nitrogen gas supply tank, wherein one end of the olefin raw material tank is communicated with the high-pressure nitrogen gas supply tank, and the other end of the olefin raw material tank is communicated with the purification test system;
the device comprises a high-pressure nitrogen gas supply tank, an olefin raw material tank, a high-pressure nitrogen gas supply tank, a circulating feed back pipe, a circulating electromagnetic valve and a circulating manual ball valve, wherein an olefin pressure sensor is arranged on a pipeline between the olefin raw material tank and the high-pressure nitrogen gas supply tank, an olefin raw material feed pump is arranged on a pipeline between the olefin raw material tank and a feed end of a purification test system, the circulating feed back pipe is arranged between the olefin raw material tank and a discharge end of the purification test system, and the circulating feed back.
Furthermore, the pretreatment system comprises a gas supply unit and a gas heater arranged between the gas supply unit and the feed end of the purification test system, wherein the gas supply unit comprises a plurality of gas cylinders respectively communicated with the gas heater;
the pipeline between the gas heater and the gas cylinder is provided with a first manual ball valve, a gas purification filter, a gas pressure sensor, a gas mass flowmeter and a second manual ball valve, and the pipeline between the gas heater and the feed end of the purification test system is provided with a third manual ball valve.
Further, the gas supply unit comprises 3 gas cylinders which are respectively high-purity N2Gas cylinder, H2/N2Gas cylinder, O2/N2A gas cylinder;
the feed end of the purification test system is provided with a feed pipe, the feed pipe and the connecting pipe are provided with a feed electromagnetic valve, a feed temperature sensor and a feed pressure sensor, and the inlet end of the purification reactor is lower than the outlet end;
the impurity analysis system comprises a gas chromatograph and a visual interface electrically connected with the gas chromatograph, wherein the visual interface can select a display or a computer and the like.
Further, the olefin storage system comprises an olefin collection tank, and a waste gas exhaust pipe and a polymerization reactor connecting pipe which are respectively communicated with the olefin collection tank, wherein a waste gas pressure regulating valve is arranged on the waste gas exhaust pipe, and a manual purification material ball valve and a purification material flow pump are arranged on the polymerization reactor connecting pipe;
and a discharge electromagnetic valve and a discharge manual ball valve are arranged on a pipeline between the discharge end of the purification test system and the olefin collecting tank.
The control system includes a PLC controller electrically connected to various pressure sensors, temperature sensors, pumps, valves, mass flow meters, gas heaters, gas purification filters, gas chromatographs, displays, and the like electrical components.
Furthermore, the purification reactor comprises an inner-layer purification reaction tube and an outer-layer constant-temperature cooling jacket arranged outside the inner-layer purification reaction tube, wherein a material inlet and a material outlet are formed in the side surface of the inner-layer purification reaction tube, and a cooling liquid inlet and a cooling liquid outlet are formed in the side surface of the outer-layer constant-temperature cooling jacket;
the top and the bottom of the inner layer purification reaction tube are respectively provided with a sealing structure, the sealing structure comprises a flange fixedly arranged on the inner layer purification reaction tube, an end cover used for sealing the end part of the inner layer purification reaction tube and a sealing ring arranged between the flange and the end cover, the flange is provided with a sealing ring positioning groove used for placing the sealing ring, the end cover is provided with a sealing ring pressing boss used for pressing the sealing ring, the flange and the end cover are detachably connected through a bolt-nut assembly, and the bolt-nut assembly comprises a bolt and a nut;
the inner layer purification reaction tube is internally provided with a first copper net layer, a lower quartz cotton layer, a second copper net layer, a purifying agent layer, a third copper net layer, an upper quartz cotton layer and a fourth copper net layer from bottom to top in sequence.
An olefin purifying agent performance efficient evaluation method based on the evaluation device comprises the following steps: and respectively filling olefin purifying agents with the same or different functions into the purifying reactors, starting the device, and evaluating the olefin purifying agents.
Further, the olefin purifying agent comprises one or more of a desulfurizing agent, a dehydrating agent, a dearsenizing agent, a carbon monoxide removing agent or a deoxidizing agent;
the desulfurizing agent comprises one or more of a desulfurizing hydrolysis catalyst for decarbonylation and desulfurization or a desulfurizing agent for removing hydrogen sulfide;
the dehydrating agent comprises one or more of alumina or molecular sieve;
the dearsenization agent comprises one or more of copper oxide-based dearsenization agent, manganese oxide-based dearsenization agent or lead oxide-based dearsenization agent;
the carbon monoxide removing agent takes copper or cobalt in an oxidation state as an active component, zinc oxide as a first auxiliary agent, and cerium oxide or zirconium oxide as a second auxiliary agent;
the deoxidizer comprises one or more of a nickel deoxidizer, a manganese deoxidizer or a copper deoxidizer.
Further, after the olefin purifying agent needing oxidation activation pretreatment is separately filled into the purification reactor, the pretreatment system provides constant temperature of 200-400 ℃ and 1-25 v/v% O2Oxidizing and activating for 1-12 hours by inert gas flow;
for the olefin purifying agent needing reduction activation pretreatment, after being separately filled into a purification reactor, the olefin purifying agent is provided with 1-10 v/v% H at constant temperature of 100-200 ℃ by a pretreatment system2Reducing and activating for 1-12 h by inert gas flow;
filling all the olefin purifying agents to be evaluated into a purifying reactor, carrying out oxidation/reduction activation pretreatment, and providing high-purity N at constant temperature of 150-400 ℃ by a pretreatment system2And (5) blowing the purification test system and the olefin purifying agent for 1-24 hours by using gas flow.
Further, when an evaluation device is utilized to simulate the purification process conditions in the actual industry, the liquid phase space velocity of the liquid phase olefin raw material passing through each purification reactor is 0.5-10.0 h at 10-30 ℃ and 1.0-10.0 MPa-1。
The evaluation device comprises an olefin raw material system capable of providing olefin materials containing impurities, a pretreatment system close to a working condition pretreatment mode, a purification test system comprising a plurality of purification reactors, an olefin storage system for storing the purified olefin materials, an impurity analysis system for collecting and analyzing the olefin materials from the purification reactors, and a control system for monitoring the operation process of the whole device in real time. Different purifying agents are put into each purifying reactor of the purifying test system; after the gas from the pretreatment system is used for carrying out activation/blowing pretreatment on each purifying agent, introducing olefin raw materials provided by the olefin raw material system into a purification test system; the olefin subjected to single or multiple circulating purification treatment obtains an analysis result by an impurity analysis system, relevant data are automatically recorded, and the purification capacity of each purifying agent is compared and improved by comparing and analyzing the content of residual impurities in the olefin; the qualified "polymer grade" olefin feed may be passed to an olefin storage system. The evaluation device has the advantages of being capable of evaluating multiple types of olefin purifiers, better in applicability and closer to working conditions.
According to the invention, the sampling pipe orifice and the sensor of the impurity analysis system are directly connected with the front end and the rear end of each purification reactor, so that different purifying agents can be applied to impurities with different concentrations, the impurity analysis system can record data changes of impurity content, temperature, pressure drop, flow and the like of olefin passing through each purifying agent bed layer in real time in the purification test process, in-situ collection of olefin materials is realized, the accuracy, the efficiency and the high applicability of the main body of the evaluation device to purification performance evaluation can be improved, and the device can be widely applied to large-scale purifying agent evaluation research.
Compared with the prior art, the invention has the following characteristics:
1) the evaluation device of the invention forms an olefin purification device platform capable of comprehensively evaluating the effects of various purifiers, the evaluation process fully simulates industrial application conditions including olefin raw material conditions, full particles of the purifiers, pretreatment conditions, purification working condition conditions and the like, and one or more types of purifiers can be flexibly selected to carry out performance evaluation;
2) the evaluation device of the invention uses a PLC control system, so that the operation process of the whole device is controllable, each system and each gas circuit in the device can be accurately controlled, key data such as temperature, pressure drop, flow and online impurity sampling analysis results in the evaluation process can be obtained and recorded, the problem that purifying agent manufacturers and purifying agent application manufacturers pay close attention to is solved, and the maximum utilization rate of the purifying agent is realized;
3) the polymer-grade olefin material evaluated by the device is introduced into the olefin collecting tank for recycling, impurities can be continuously added for a purification evaluation test, and a pure olefin raw material can be provided for a downstream polyolefin preparation test, so that the cost of a large amount of raw materials can be saved, and the pollution caused by directly discharging a large amount of olefin into a waste gas pipeline can be avoided;
4) the evaluation device is simple in design, can realize the operation of an automatic control system through an external control computer, can also carry out manual adjustment, and is high in practicability and flexibility and convenient to popularize.
Drawings
FIG. 1 is a schematic view showing the overall structure of a purification apparatus according to the present invention;
FIG. 2 is a schematic view of the structure of the purification reactor of the present invention.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
Example 1:
an evaluation device as shown in fig. 1 and 2 is preferably but not limited to be used as a purification evaluation device for propylene. The evaluation device comprises an olefin raw material system, a pretreatment system, a purification test system, an olefin storage system, an impurity analysis system and a control system.
Providing propylene material containing impurities from olefin material system, placing liquid phase propylene material in 50L olefin material tank 1-1, connecting high pressure nitrogen gas supply tank 1-2 at front end of olefin material tank 1-1, and providing N above 2MPa2The pressure is kept to be higher than 1MPa all the time in the olefin raw material tank 1-1 and is monitored by an olefin pressure sensor 1-3 so as to ensure that the propylene material is in a liquid phase state all the time in the tank; the rear end of an olefin raw material tank 1-1 is connected with an olefin raw material discharging pipe which is directly communicated with the bottom, the rear end of the olefin raw material discharging pipe is connected with a numerical control olefin raw material feeding pump 1-4, the outlet flow rate of propylene materials is set, an outlet switch of the olefin raw material feeding pump 1-4 is opened, and finally the olefin raw material discharging pipe is communicated with a rear end purification test systemAnd (4) a system. The olefin pressure sensor 1-3 and the olefin raw material feeding pump 1-4 are connected with a control system, and can be monitored by software or manually operated and observed.
The propylene material containing impurities is introduced into a purification test system, the purification test system consists of four purification reactors (A, B, C, D) which are connected in series and can be filled with different purifying agents and parts, and a desulfurizing agent, a dehydrating agent, an arsenic removing agent and a carbon monoxide removing agent in the prior art are selected and sequentially filled into the four purification reactors in sequence. The propylene material containing impurities at the outlet of the olefin raw material system flows through a pipeline provided with a feeding temperature sensor 3-2 and a feeding pressure sensor 3-3 through an opened feeding electromagnetic valve 3-1 and then is introduced into a desulfurizer bed layer of the A purification reactor from bottom to top from an inlet at the lower end of the A purification reactor through a feeding pipe 3-4 to finish H2And (5) purifying and removing S. The propylene material at the outlet at the upper end of the A purification reactor is connected with the inlet at the lower end of the B purification reactor through an opened electromagnetic valve, a temperature sensor, a pressure sensor and the like, and is introduced into the dehydrating agent bed layer of the B purification reactor from bottom to top to finish H2And deeply purifying and removing O. The propylene material at the outlet of the upper end of the B purification reactor is connected with the inlet of the lower end of the C purification reactor through an opened electromagnetic valve, a temperature sensor, a pressure sensor and the like, and is introduced into the dearsenization agent bed layer of the C reaction reactor from bottom to top to complete the purification and removal of As compounds. The propylene material at the outlet of the upper end of the C purification reactor is connected with the inlet of the lower end of the D purification reactor through an opened electromagnetic valve, a temperature sensor, a pressure sensor and the like, and is introduced into the carbon monoxide removal agent bed layer of the D reaction purifier from bottom to top to complete the deep purification and removal of CO. And the outlet at the upper end of the purification reactor is connected with three paths through a plurality of three-way joints, the first path is a sampling pipeline 3-10 and leads to an impurity analysis system, the second path is sequentially connected with a discharge electromagnetic valve 3-11 and a discharge manual ball valve 3-12 and finally leads to an olefin storage system, and the third path is sequentially connected with a circulation electromagnetic valve 3-13, a circulation manual ball valve 3-14 and a circulation feed back pump and finally returns to an olefin raw material tank 1-1 through a circulation feed back pipe 3-15. Wherein, the related pipelines are provided with locking nuts, metal washers, sealing rings, bent pipe metal joints and other parts; the electromagnetic valve, the temperature sensor and the pressure sensorAll the devices and the like are connected with a control system, can be monitored by software, and can also be manually operated, observed and operated.
The impurity analysis system is respectively connected with five sampling pipelines (3-5, 3-7, 3-8, 3-9 and 3-10) at the inlet and outlet ports of each purification reactor (A, B, C, D), the online collection of materials at the inlet end and the outlet end of each purification reactor is realized by controlling a pneumatic valve 5-1 on each sampling pipeline, a single or a plurality of parallel multifunctional gas chromatographs 5-2 at the rear end are introduced through PLC control, the analysis data of the impurity content detected in olefin is transmitted to a visual interface 5-3 controlled by a control system, the corresponding impurity content change after passing through each purifying agent bed is compared, and finally whether the purified propylene material meets the requirement of polymerization grade propylene is evaluated.
Example 2:
and on a visual interface 5-3, data changes of impurity content, temperature, pressure drop, flow and the like before and after the propylene passes through each purifying agent bed layer are recorded in real time, so that the accuracy, the efficiency and the high applicability of the evaluation device to the performance evaluation of the purifying agents are improved.
In the embodiment, different purifying agents are applied to impurities with different concentrations, and an impurity analysis system is used for recording data changes of impurity content, temperature, pressure drop and the like before and after propylene passes through each purifying agent bed layer in real time in the purification test process, wherein the types and the contents of toxic substances contained in different olefin raw materials in the industry are different, and the applied plant working condition conditions are also different, and the test results 1-4 in the table 1 show that.
TABLE 1 results of experimental evaluation of impurity removal of various purifiers
Example 3:
and (3) detecting by an impurity analysis system, and when the content of various impurities in the purified propylene is lower than the requirement of polymerization-grade propylene, determining the propylene as a qualified propylene material. Opening a discharge electromagnetic valve 3-11 and a discharge manual ball valve 3-12 which are connected with the purification testing system, and introducing qualified propylene into an olefin collecting tank 4-1 in an olefin storage system. When liquid phase propylene is slowly introduced into the olefin collecting tank 4-1, the waste gas pressure regulating valve 4-2 with the rear end controlled by the PLC is opened, the lowest opening pressure of the waste gas pressure regulating valve 4-2 is set to be 1.1-1.5 MPa, the propylene in the tank is ensured to be in a liquid phase state when stored, and a pipeline behind the waste gas pressure regulating valve 4-2 is connected with a waste gas discharge and collection system. The rear end of the other pipeline is connected with a manual purification material ball valve 4-3 and a purification material flow pump 4-4, and finally connected with a pipeline leading to the polypropylene polymerization reactor. When the impurity content in the purified propylene material is lower than the impurity requirement of the polymerization grade propylene, the propylene material records the impurity content and can be collected in the olefin collecting tank 4-1 for downstream preparation of the polypropylene or be mixed with the impurity again to serve as a propylene raw material for the next test.
Example 4:
after the detection of the impurity analysis system, if the content of various impurities in the purified propylene is still higher than the impurity requirement of the "polymer grade" propylene, the purified propylene is regarded as an unqualified material, and the purified propylene can be continuously introduced into the olefin collection tank 4-1 as in example 3 or subjected to recycling purification again. And opening a circulating electromagnetic valve 3-13, a circulating manual ball valve 3-14 and a circulating feed back pump which are connected with a third pipeline at the discharge end in the purification test system, setting a certain flow rate for the circulating feed back pump, returning the circulating feed back pump into the olefin raw material tank 1-1 from the bottom after passing through the circulating feed back pipe 3-15, and carrying out a secondary purification test as in example 1 until the impurity requirement of polymerization-grade propylene is met.
Example 5:
the key core of the purification test system is the purification reactor (A-D) which comprises an inner layer purification reaction tube J-1 and an outer layer constant temperature cooling jacket J-2, as shown in detail in FIG. 2. The inner layer purification reaction tube J-1 is made of stainless steel, the side surface of the lower end is a material inlet J-3 of propylene materials, and the side surface of the upper end is a material outlet J-4 of the propylene materials; the inner diameter of the inner layer purification reaction tube J-1 is 9cm, the outer diameter is 12-16cm, the length is about 55-60 cm, and the height of an effective filling bed layer is 50 cm. In order to ensure the pressure of the purification reaction, the upper end and the lower end of the inner layer purification reaction tube J-1 are provided with sealing structures which comprise an end cover J-5, a sealing ring J-6, a flange J-7 welded on the inner layer purification reaction tube J-1, a bolt J-8 and a nut J-9. The outer constant temperature cooling jacket J-2 is a stainless steel jacket with built-in cooling liquid, and is connected with a refrigeration circulator capable of setting the temperature range of-10 ℃ to 50 ℃, and the cooling liquid circulates in the stainless steel jacket and is used for assisting in stabilizing the purification reaction temperature.
One to four of desulfurizer, dehydrating agent, dearsenization agent, carbon monoxide removal and deoxidizing agent in the prior art are selected, and the filling of key purifying agent is started. The purifying agent in the embodiment is selected, weighed and filled in the following modes: firstly, respectively measuring 1.5L of alumina-titania-based hydrolytic desulfurizer, 1.5L of zinc oxide-based desulfurizer, 3L of mixed dehydrating agent of molecular sieve and alumina, 3L of dearsenization agent mainly containing copper, manganese and lead metal oxide and 3L of carbon monoxide removal agent mainly containing copper, zinc and cerium metal oxide according to bulk density; respectively laying a copper net at the bottoms of the four inner-layer purification reaction tubes J-1, padding a layer of quartz cotton with the thickness of about 1-2 cm on the copper net, and laying a copper net; filling 1.5L of desulfurizer into the purification reactor by a tight stack method, slightly knocking the tube wall to ensure that the sample is tightly filled, then pouring 1.5L of desulfurizer into the purification reactor, and slightly knocking the tube wall; similarly, 3L of dehydrating agent is filled in the purifying reactor B by a close-packed method, 3L of dearsenic agent is filled in the purifying reactor C, and 3L of carbon monoxide removing agent is filled in the purifying reactor D; and finally, paving a copper net on each purifying agent, filling a layer of quartz cotton with the thickness of about 1-2 cm, paving another copper net, finally placing a sealing ring J-6, covering an end cover J-5, screwing a fixing flange J-7 and the end cover J-5 through a bolt J-8 and a nut J-9, ensuring sealing, and finishing filling of the purifying agent.
Under the condition of equipping the core purification reactor, the evaluation device can directly simulate the purification process conditions in the actual industry, and the liquid-phase propylene raw material is introduced under the conditions of normal temperature of 10-30 ℃ and pressure of 1.0-5.0 MPaThe liquid phase airspeed of the liquid phase passing through each purification bed layer is 0.5-5.0 h-1And the purifying ability of each purifying agent was evaluated in accordance with the method of example 1.
Example 6:
according to the evaluation conducted in example 1, each purification reactor may be filled with a different functional purification agent, and the impurity purification performance of a certain purification agent can be evaluated as a whole or individually, and the purification agent to be filled may be a molded desulfurization agent, a dehydrating agent, a dearsenization agent, a carbon monoxide removal agent, a deoxidizer. However, because part of the catalyst such as part of copper-based decarbonization and copper-based deoxidizer needs to be reduced and treated, part of the cobalt-based decarbonization and oxidation pretreatment is needed, and all the purifiers need to be subjected to N before purification evaluation2And (3) high-temperature blowing pretreatment, wherein all the pretreatment aims to strengthen the activity of a purifying agent and reduce the adsorption of surface impurities on polluted raw materials.
The evaluation apparatus of example 1, the pretreatment system thereof comprised a gas supply unit and gas heaters 2 to 9. The gas supply unit includes supplying high purity N separately2Containing 10% of H2/N2Containing 5% of O2/N2The gas cylinders (2-1 to 2-3) are connected with the gas supply units in series in sequence, a first manual ball valve 2-4 for opening or closing a gas circuit, a gas purification filter 2-5, a gas pressure sensor 2-6, a gas mass flow meter 2-7 for measuring the flow rate of the gas circuit and a second manual ball valve 2-8 for opening or blocking the circulation of the gas circuit inside and outside the gas distribution system are connected with the gas heater 2-9 finally; the gas pressure sensors 2-6 and the gas mass flow meters 2-7 are connected with a control system, and can be monitored by software or visually observed. The enhanced heating mixer 2-9 is connected with the air outlet end of the air supply unit, the air outlet end and the air inlet end of the enhanced heating mixer 2-9 are respectively internally provided with a temperature sensor, and the temperature sensors are connected with a control system.
Using the scavenger selected in example 5 as an example, a reduction/pretreatment operation was carried out. First, the copper-based carbon monoxide remover was charged into the D purification reactor in the same manner as in example 5, and high purity N was opened2Gas cylinder 2-1, 10% H2/N2The gas cylinder 2-2 is opened and closed, and the first manual ball valve 2-4 and the second manual ball valve in the corresponding gas path are openedAnd the movable ball valve 2-8 and the third manual ball valve 2-10 are sequentially connected with the gas purification filter 2-5, the gas pressure sensor 2-6 and the gas mass flowmeter 2-7 and finally connected with the gas heater 2-9 to perform gas heating and mixing. The control system sets corresponding gas flow and heating temperature of the gas heater 2-9 to ensure that the flow of the mixed gas at the outlet is 200h-1～500h-15% H at 160-200 DEG C2/N2. Wherein, the real-time data of the temperature sensors at the gas outlet end and the gas inlet end of the gas pressure sensor 2-6, the gas mass flow meter 2-7 and the gas heater 2-9 which are connected with the control system can be visually observed. The carbon monoxide removal purifying agent flows for 200 hours-1～500h -15% H at 160-200 DEG C2/N2And after about 4-8 h of reduction, the activation is finished, all valves of the gas circuit of the pretreatment system are closed, and valves in front of and behind the D purification reactor are closed, so that no air enters.
Then, the desulfurizing agent, the dehydrating agent and the dearsenizing agent are sequentially filled into the A-C purifying reactors according to the filling method of the embodiment 5, and after the filling is finished, the high-purity N is opened2And opening a first manual ball valve 2-4, a second manual ball valve 2-8 and a third manual ball valve 2-10 in a corresponding gas path, sequentially passing through a gas purification filter 2-5, a gas pressure sensor 2-6 and a gas mass flowmeter 2-7, and finally connecting with a gas heater 2-9 to perform gas heating and mixing, wherein the gas bottle 2-1 is opened. The control system sets corresponding gas flow and heating temperature of the gas heater 2-9 to ensure that the flow of the mixed gas at the outlet is 200h-1～500h-1High purity N at 300-400 DEG C2. All the purifying agent beds pass through for 200 hours-1～500h-1High purity N at 300-400 DEG C2And after purging for about 4-8 h, finishing pretreatment, closing all valves of a pretreatment system, and closing valves in front of and behind the A-D purification reactors before carrying out an olefin purification evaluation test to ensure that no air enters. Finally, the decontamination evaluation was carried out by the evaluation apparatus according to examples 1 to 3.
Example 7:
an evaluation device capable of simulating the purification capacity of various purifiers on multi-component impurities in an olefin raw material under actual working conditions comprises an olefin raw material system, a pretreatment system, a purification test system, an olefin storage system, an impurity analysis system and a control system. Different purifying agents are placed in each purifying reactor of the purification test system, after the gas from the pretreatment system activates/purges each purifying agent, the propylene raw material provided by the olefin raw material system is introduced into the purification test system, the propylene after single or multiple circulation purification treatment is tested by the impurity analysis system, the content of residual impurities in the propylene is contrastively analyzed, the purification capacity of each purifying agent is compared and improved, and meanwhile, the qualified 'polymer grade' propylene material can be introduced into the olefin storage system.
Specifically, as shown in fig. 1, the evaluation device for efficiently evaluating the performance of the olefin purification agent comprises an olefin raw material system, a pretreatment system, a purification test system, an impurity analysis system, an olefin storage system and a control system, wherein the purification test system comprises a plurality of purification reactors which are sequentially connected in series and used for filling olefin purification agents with the same or different functions, a connecting pipe 3-6 communicated with the impurity analysis system is arranged between every two adjacent purification reactors, the feed end of the purification test system is respectively communicated with the olefin raw material system, the pretreatment system and the impurity analysis system, the discharge end of the purification test system is respectively communicated with the impurity analysis system and the olefin storage system, and the control system is respectively electrically connected with the olefin raw material system, the pretreatment system, the purification test system, the impurity analysis system and the olefin storage system.
The olefin raw material system comprises an olefin raw material tank 1-1 and a high-pressure nitrogen gas supply tank 1-2, wherein one end of the olefin raw material tank 1-1 is communicated with the high-pressure nitrogen gas supply tank 1-2, and the other end of the olefin raw material tank is communicated with the purification test system; an olefin pressure sensor 1-3 is arranged on a pipeline between an olefin raw material tank 1-1 and a high-pressure nitrogen gas supply tank 1-2, an olefin raw material feed pump 1-4 is arranged on a pipeline between the olefin raw material tank 1-1 and a feed end of a purification test system, a circulating return pipe 3-15 is arranged between the olefin raw material tank 1-1 and a discharge end of the purification test system, and a circulating return pump, a circulating electromagnetic valve 3-13 and a circulating manual ball valve 3-14 are arranged on the circulating return pipe 3-15.
The pretreatment system comprises a gas supply unit and gas heaters 2-9 arranged between the gas supply unit and the feed end of the purification test system, wherein the gas supply unit comprises a plurality of gas cylinders respectively communicated with the gas heaters 2-9; a first manual ball valve 2-4, a gas purification filter 2-5, a gas pressure sensor 2-6, a gas mass flowmeter 2-7 and a second manual ball valve 2-8 are arranged on a pipeline between the gas heater 2-9 and the gas bottle, and a third manual ball valve 2-10 is arranged on a pipeline between the gas heater 2-9 and the feed end of the purification test system.
A feeding pipe 3-4 is arranged at the feeding end of the purification test system, and a feeding electromagnetic valve 3-1, a feeding temperature sensor 3-2 and a feeding pressure sensor 3-3 are arranged on the feeding pipe 3-4 and a connecting pipe 3-6; the inlet end of the purification reactor is lower than the outlet end.
The impurity analysis system includes a gas chromatograph 5-2 and a visualization interface 5-3 electrically connected to the gas chromatograph 5-2.
The olefin storage system comprises an olefin collection tank 4-1, and a waste gas exhaust pipe 4-5 and a polymerization reactor connecting pipe 4-6 which are respectively communicated with the olefin collection tank 4-1, wherein a waste gas pressure regulating valve 4-2 is arranged on the waste gas exhaust pipe 4-5, and a purified material manual ball valve 4-3 and a purified material flow pump 4-4 are arranged on the polymerization reactor connecting pipe 4-6; a discharge electromagnetic valve 3-11 and a discharge manual ball valve 3-12 are arranged on a pipeline between the discharge end of the purification test system and the olefin collecting tank 4-1.
As shown in FIG. 2, the purification reactor comprises an inner-layer purification reaction tube J-1 and an outer-layer constant-temperature cooling jacket J-2 arranged outside the inner-layer purification reaction tube J-1, wherein a material inlet J-3 and a material outlet J-4 are arranged on the side surface of the inner-layer purification reaction tube J-1, and a cooling liquid inlet J-11 and a cooling liquid outlet J-10 are arranged on the side surface of the outer-layer constant-temperature cooling jacket J-2; the top and the bottom of the inner layer purification reaction tube J-1 are respectively provided with a sealing structure, the sealing structures comprise a flange J-7 fixedly arranged on the inner layer purification reaction tube J-1, an end cover J-5 used for sealing the end part of the inner layer purification reaction tube J-1 and a sealing ring J-6 arranged between the flange J-7 and the end cover J-5, the flange J-7 is provided with a sealing ring positioning groove J-12 used for placing the sealing ring J-6, the end cover J-5 is provided with a sealing ring pressing boss J-13 used for pressing the sealing ring J-6, the flange J-7 and the end cover J-5 are detachably connected through a bolt and nut assembly, and the bolt and nut assembly comprises a bolt J-8 and a nut J-9; the inner layer purification reaction tube J-1 is internally provided with a first copper net layer, a lower quartz cotton layer, a second copper net layer, a purifying agent layer, a third copper net layer, an upper quartz cotton layer and a fourth copper net layer from bottom to top in sequence.
The efficient evaluation method of the performance of the olefin purifying agent based on the evaluation device comprises the following steps: and respectively filling olefin purifying agents with the same or different functions into the purifying reactors, starting the device, and evaluating the olefin purifying agents. Wherein, aiming at propylene materials containing different impurities, different functional purifiers can be filled in each purifying reactor to integrally or individually evaluate the impurity purifying performance of a certain purifier.
The filling purifying agent can be formed desulfurizer, dehydrating agent, dearsenization agent, carbon monoxide removing agent and deoxidant. Wherein:
(1) as the desulfurizing agent, a desulfurizing hydrolysis catalyst for COS (carbonyl sulfide) and dehydrogenation catalyst for H were evaluated2The desulfurizing agent of S (hydrogen sulfide) is prepared by modifying a hydrolysis catalyst with alumina base or alumina-titania base by soaking alkali metal and other components, and mainly adding zinc oxide and a promoter component and a binder. The desulfurization hydrolysis catalyst can be provided with a zinc oxide desulfurizer and is serially connected in one purification reactor for test evaluation, or is singly filled in two purification reactors for test evaluation.
(2) The estimated dehydrating agents were mainly alumina and molecular sieves.
(3) The estimated dearsenization agent is mainly prepared by adding a catalytic component and a binder into copper oxide base, manganese oxide base and lead oxide base.
(4) The estimated CO removing agent is prepared by taking oxidized copper, cobalt or nickel as an active component and adding an auxiliary agent component and graphite.
(5) The deoxidizers that can be evaluated are mainly nickel-based deoxidizers, manganese-based deoxidizers, and copper-based deoxidizers.
(6) The oxygenate can be evaluated as a molecular sieve or as a complex with a molecular sieve as the major active ingredient.
The evaluation device needs to be pretreated and reevaluated after filling the purifying agent, and the pretreatment process comprises the following steps:
(1) for various purificant needing oxidation activation pretreatment, after being separately filled into a purification reactor, the purificant can be provided with 1-25 v/v% O at constant temperature of 200-400 ℃ by a pretreatment system2And/inert gas flow, and oxidizing and activating for 1-12 hours.
(2) For various purificant needing reduction activation pretreatment, the purificant can be independently filled into a purification reactor, and then a pretreatment system provides constant temperature of 100-200 ℃ and H with concentration of 1-10 v/v%2And/or carrying out reduction activation for 1-12 h by using inert gas flow.
(3) The purifying agent to be evaluated is fully filled into the purifying reactor, and after necessary oxidation/reduction pretreatment, the pretreatment system provides high-purity N with constant temperature of 150-400 DEG C2And (5) gas flowing, and purging the whole purification test system and the purifying agent for 1-24 hours.
When the evaluation device is used for simulating purification process conditions in actual industry, the liquid phase olefin raw material passes through each purification reactor at the temperature of 10-30 ℃ and the pressure of 1.0-10.0 MPa, and the liquid phase space velocity is 0.5-10.0 h-1。
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. The evaluation device for efficiently evaluating the performance of the olefin purifying agent is characterized by comprising an olefin raw material system, a pretreatment system, a purification test system, an impurity analysis system, an olefin storage system and a control system, wherein the purification test system comprises a plurality of purification reactors which are sequentially connected in series and used for filling the olefin purifying agents with the same or different functions, a connecting pipe (3-6) communicated with the impurity analysis system is arranged between every two adjacent purification reactors, the feed end of the purification test system is respectively communicated with the olefin raw material system, the pretreatment system and the impurity analysis system, the discharge end of the purification test system is respectively communicated with the impurity analysis system and the olefin storage system, and the control system is respectively communicated with the olefin raw material system, the pretreatment system, the purification test system, the impurity analysis system, the olefin storage system, The olefin storage system is electrically connected.
2. The apparatus for evaluating olefin purification performance with high efficiency according to claim 1, wherein the olefin feed system comprises an olefin feed tank (1-1) and a high pressure nitrogen gas supply tank (1-2), one end of the olefin feed tank (1-1) is communicated with the high pressure nitrogen gas supply tank (1-2), and the other end is communicated with the purification test system;
the device is characterized in that an olefin pressure sensor (1-3) is arranged on a pipeline between the olefin raw material tank (1-1) and the high-pressure nitrogen gas supply tank (1-2), an olefin raw material feed pump (1-4) is arranged on a pipeline between the olefin raw material tank (1-1) and the feed end of the purification test system, a circulating material return pipe (3-15) is arranged between the olefin raw material tank (1-1) and the discharge end of the purification test system, and a circulating material return pump, a circulating electromagnetic valve (3-13) and a circulating manual ball valve (3-14) are arranged on the circulating material return pipe (3-15).
3. The evaluation device for efficiently evaluating the performance of an olefin purification agent according to claim 1, wherein the pretreatment system comprises a gas supply unit and gas heaters (2-9) arranged between the gas supply unit and the feed end of the purification test system, the gas supply unit comprises a plurality of gas cylinders respectively communicated with the gas heaters (2-9);
a first manual ball valve (2-4), a gas purification filter (2-5), a gas pressure sensor (2-6), a gas mass flowmeter (2-7) and a second manual ball valve (2-8) are arranged on a pipeline between the gas heater (2-9) and the gas cylinder, and a third manual ball valve (2-10) is arranged on a pipeline between the gas heater (2-9) and the feed end of the purification test system;
the gas supply unit comprises 3 gas cylinders which are respectively high-purity N2Gas cylinder (2-1), H2/N2Gas cylinder (2-2), O2/N2And gas cylinders (2-3).
4. The evaluation device for efficiently evaluating the performance of the olefin purifier according to claim 1, wherein a feed pipe (3-4) is arranged at the feed end of the purification test system, a feed electromagnetic valve (3-1), a feed temperature sensor (3-2) and a feed pressure sensor (3-3) are arranged on the feed pipe (3-4) and a connecting pipe (3-6), and the inlet end of the purification reactor is lower than the outlet end;
the impurity analysis system comprises a gas chromatograph (5-2) and a visual interface (5-3) electrically connected with the gas chromatograph (5-2).
5. The device for efficiently evaluating the performance of the olefin purifier according to claim 1, wherein the olefin storage system comprises an olefin collection tank (4-1), an exhaust gas exhaust pipe (4-5) and a polymerization reactor connecting pipe (4-6), the exhaust gas exhaust pipe (4-5) is respectively communicated with the olefin collection tank (4-1), an exhaust gas pressure regulating valve (4-2) is arranged on the exhaust gas exhaust pipe (4-5), and a purified material manual ball valve (4-3) and a purified material flow pump (4-4) are arranged on the polymerization reactor connecting pipe (4-6);
and a discharge electromagnetic valve (3-11) and a discharge manual ball valve (3-12) are arranged on a pipeline between the discharge end of the purification test system and the olefin collecting tank (4-1).
6. The evaluation device for efficiently evaluating the performance of the olefin purifier according to claim 1, wherein the purification reactor comprises an inner-layer purification reaction tube (J-1) and an outer-layer constant-temperature cooling jacket (J-2) arranged outside the inner-layer purification reaction tube (J-1), the side surface of the inner-layer purification reaction tube (J-1) is provided with a material inlet (J-3) and a material outlet (J-4), and the side surface of the outer-layer constant-temperature cooling jacket (J-2) is provided with a cooling liquid inlet (J-11) and a cooling liquid outlet (J-10);
the top and the bottom of the inner layer purification reaction tube (J-1) are respectively provided with a sealing structure, the sealing structures comprise a flange (J-7) fixedly arranged on the inner layer purification reaction tube (J-1), an end cover (J-5) used for sealing the end part of the inner layer purification reaction tube (J-1) and a sealing ring (J-6) arranged between the flange (J-7) and the end cover (J-5), the flange (J-7) is provided with a sealing ring positioning groove (J-12) used for placing the sealing ring (J-6), the end cover (J-5) is provided with a sealing ring pressing boss (J-13) used for pressing the sealing ring (J-6), and the flange (J-7) and the end cover (J-5) are detachably connected through a bolt and nut component, the bolt and nut assembly comprises a bolt (J-8) and a nut (J-9);
the inner layer purification reaction tube (J-1) is internally provided with a first copper net layer, a lower quartz cotton layer, a second copper net layer, a purifying agent layer, a third copper net layer, an upper quartz cotton layer and a fourth copper net layer from bottom to top in sequence.
7. An olefin scavenger performance efficient evaluation method based on the evaluation apparatus according to any one of claims 1 to 6, characterized in that the method comprises: and respectively filling olefin purifying agents with the same or different functions into the purifying reactors, starting the device, and evaluating the olefin purifying agents.
8. The method for efficiently evaluating the performance of an olefin purification agent based on an evaluation device as claimed in claim 7, wherein the olefin purification agent comprises one or more of a desulfurizing agent, a dehydrating agent, an arsenic removing agent, a carbon monoxide removing agent or a deoxidizing agent;
the desulfurizing agent comprises one or more of a desulfurizing hydrolysis catalyst for decarbonylation and desulfurization or a desulfurizing agent for removing hydrogen sulfide;
the dehydrating agent comprises one or more of alumina or molecular sieve;
the dearsenization agent comprises one or more of copper oxide-based dearsenization agent, manganese oxide-based dearsenization agent or lead oxide-based dearsenization agent;
the carbon monoxide removing agent takes copper or cobalt in an oxidation state as an active component, zinc oxide as a first auxiliary agent and cerium oxide or zirconium oxide as a second auxiliary agent;
the deoxidizer comprises one or more of a nickel deoxidizer, a manganese deoxidizer or a copper deoxidizer.
9. The method for efficiently evaluating the performance of an olefin purifier based on an evaluation device according to claim 7,
for the olefin purifying agent needing oxidation activation pretreatment, after being separately filled into a purification reactor, the olefin purifying agent is provided with 1-25 v/v% O at constant temperature of 200-400 ℃ by a pretreatment system2Oxidizing and activating for 1-12 hours by inert gas flow;
for the olefin purifying agent needing reduction activation pretreatment, after being separately filled into a purification reactor, the olefin purifying agent is provided with 1-10 v/v% H at constant temperature of 100-200 ℃ by a pretreatment system2Reducing and activating for 1-12 h by inert gas flow;
filling all the olefin purificant to be evaluated into a purification reactor, carrying out oxidation/reduction activation pretreatment, and providing high-purity N at constant temperature of 150-400 ℃ by a pretreatment system2And (5) blowing the purification test system and the olefin purifying agent for 1-24 hours by using gas flow.
10. The method for efficiently evaluating the performance of the olefin purifying agent based on the evaluation device as claimed in claim 7, wherein the evaluation device is used for simulating purification process conditions in the actual industry, and the liquid phase space velocity of the liquid phase olefin raw material passing through each purification reactor is 0.5-10.0 h at 10-30 ℃ and 1.0-10.0 MPa-1。
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