CN112973593B - Method for rapidly judging driving state of gas-phase polyolefin production device - Google Patents
Method for rapidly judging driving state of gas-phase polyolefin production device Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 26
- 229920000098 polyolefin Polymers 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 59
- 239000003054 catalyst Substances 0.000 claims abstract description 34
- 239000007791 liquid phase Substances 0.000 claims abstract description 18
- 239000012071 phase Substances 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 239000002685 polymerization catalyst Substances 0.000 claims abstract description 9
- 238000001514 detection method Methods 0.000 claims abstract description 7
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 claims description 24
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 claims description 12
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 12
- 239000011651 chromium Substances 0.000 claims description 12
- 229910052804 chromium Inorganic materials 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 3
- -1 polyethylene Polymers 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 239000000178 monomer Substances 0.000 abstract description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 18
- 230000000977 initiatory effect Effects 0.000 abstract description 12
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 9
- 239000002699 waste material Substances 0.000 abstract description 5
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 238000006902 nitrogenation reaction Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 31
- 229910052799 carbon Inorganic materials 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 238000007872 degassing Methods 0.000 description 5
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 4
- 229920005672 polyolefin resin Polymers 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000006384 oligomerization reaction Methods 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
- 239000004743 Polypropylene Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229920001903 high density polyethylene Polymers 0.000 description 1
- 239000004700 high-density polyethylene Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 239000012968 metallocene catalyst Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/002—Avoiding undesirable reactions or side-effects, e.g. avoiding explosions, or improving the yield by suppressing side-reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F110/00—Homopolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F110/02—Ethene
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention discloses a method for rapidly judging the driving state of a gas-phase polyolefin production device. The technical scheme of the invention is as follows: whether the polymerization catalyst initiates the polymerization reaction is judged by detecting whether the oligomer collecting tank collects the liquid phase in the oligomer deep cooling collecting system, and the severity of the polymerization reaction initiated by the polymerization catalyst is judged by detecting the liquid level change rate of the oligomer collecting tank. The method can realize rapid detection and real-time monitoring of the polymerization reaction initiation condition at the initial stage of polyolefin process start, accurately predict the reaction process and timely adjust the catalyst addition amount to ensure the safety of start, and prevent polymerization accidents caused by excessive initiation or large waste of nitrogen and polymerization monomers caused by no initiation of the catalyst.
Description
Technical Field
The present invention relates to a method for judging the initial polymerization state of a polymer resin, and more particularly to a method for judging the driving state of a polyolefin production apparatus.
Background
At present, in the initial start-up stage of a gas phase method fluidized bed polyolefin process, the judgment of the polymerization initiation conditions of Ziegler catalysts and metallocene catalysts which have no reaction induction period and stable activity release is determined according to the changes of operating parameters such as material level, temperature, pressure and the like of a fluidized bed reactor, and the method is effective because the parameters can obviously change in a short time and can reflect the polymerization initiation conditions of the catalysts in real time. In addition, the chromium-based catalyst has a relatively long induction period for initiating a polymerization reaction, the release of the activity of the catalyst is a trend of gradually increasing, generally, the reaction parameters are obviously changed for about five or six hours, the delay of the judgment can seriously waste materials for starting the reactor, the reactor is seriously operated by mistake in serious conditions, the reaction process cannot be accurately predicted, the catalyst addition amount is not adjusted timely, the polymerization accident is caused by excessive or no polymerization reaction, and the safety of starting the reactor is seriously damaged. At present, enterprises adopt gas chromatography to detect the content of low-carbon olefin in the circulating gas of the reactor (CN 102453153B) to solve the problem. However, as the main components of the circulating gas in the reactor are polymerized monomers and hydrogen, and the activity of the chromium-based catalyst at the initial start-up stage is low, the detection of trace low-carbon olefin in the circulating gas by the gas chromatography is generally about two hours after the start-up, the detection is relatively lagged, the liquid low-carbon olefin can be rapidly collected by the cryogenic enrichment effect on the reaction exhaust gas, and even if the low-carbon olefin generated at the initial start-up stage is very trace, whether the polymerization reaction occurs can be judged by detecting whether the cryogenic liquid phase is discharged.
Disclosure of Invention
The invention aims to provide a method for quickly and effectively judging the driving state of a polyolefin production device, which can judge the condition of initiating a polymerization reaction in a short time after the driving of a catalytic reaction, adjust the adding amount of a catalyst and reduce the discharge waste of nitrogen and a polymerization monomer.
The technical scheme of the invention is as follows: a method for judging the running state of a gas-phase polyolefin production device comprises introducing a stream of circulating gas of a polymerization reaction system into an oligomer cryogenic capture system, collecting liquid-phase oligomers after cryogenic treatment, and discharging the residual gas-phase stream to a torch for treatment.
The specific gas-phase polyolefin production and exhaust gas recovery process is shown in figure 1, under normal working conditions, polymeric monomers and hydrogen enter a polyolefin fluidized bed reactor for polymerization after being pressurized by a compressor and cooled by a cooler, unreacted gas-phase polymeric monomers and hydrogen circularly flow into the compressor from the top of the reactor, polyolefin resin generated by the reaction flows out of the bottom of the reactor, enters a storage bin, and is conveyed by conveying gas into a degassing bin, and the polyolefin resin is devolatilized in the degassing bin. Fresh nitrogen is fed from the lateral line of the degassing bin, unreacted low-carbon hydrocarbon and gas-phase oligomer in the polyolefin resin are blown away, the polyolefin resin is discharged from the bottom of the degassing bin, gas is discharged from the top of the degassing bin and enters a compression and condensation unit, the gas is subjected to one-stage or multi-stage compression, condensation and gas-liquid separation, high-carbon recovery liquid is separated and returned to a polymerization reactor, the residual gas enters an oligomer cryogenic trapping system, the lowest temperature is set to be-20 ℃ to-60 ℃, the oligomer is liquefied and condensed, the oligomer is collected, a gas-phase stream flows into an expansion cryogenic unit, and polymerized monomers and nitrogen are separated through a cryogenic plate type heat exchanger and an expander, so that the nitrogen and the polymerized monomers are recycled.
In the initial start-up stage, the polymerization reactor and the reaction circulation line are usually only opened, and the detection is relatively difficult in the gas phase because of the low content of the produced oligomers. In the invention, an existing oligomer cryogenic trapping system is utilized in a driving stage, one stream is led out to enter the oligomer cryogenic trapping system, cold energy is provided by liquid nitrogen, liquid-phase oligomers are collected after cryogenic treatment, and the residual gas-phase stream is discharged to a torch. The oligomer cryogenic capture system comprises one or more stages of oligomer condensers, one or more stages of droplet coalescers, and an oligomer collection tank. The outlet temperature of the oligomer condenser was set to-20 ℃ to-30 ℃. Whether the polymerization catalyst initiates a polymerization reaction is judged by detecting whether a liquid-phase substance is collected by a oligomer collecting tank in an oligomer deep cooling collecting system, wherein the main components of the liquid-phase oligomer are 1-butene and 1-hexene. The intensity of the polymerization reaction initiated by the polymerization catalyst is judged by detecting the liquid level change rate of the oligomer collecting tank.
The preparation of polyolefins such as polyethylene and polypropylene usually employs chromium-based catalysts as the main catalytic system, which can initiate the production of 1-butene and 1-hexene. The production of 1-butene and 1-hexene can only be from Cr3+When detecting the existence of 1-butene and 1-hexene in the circulating gas, the chromium-based catalyst starts to generate activity, and the polymerization reaction of the polymerized monomer is ensured to simultaneously occur in the system, namely the catalyst already starts to initiate the polymerization of the polymerized monomer to generate polyolefin. And the 1-butene, 1-hexene and other oligomers and polymerization monomers in the circulating gas of the reactor have certain difference in condensation temperature. Based on the above theoretical analysis, if the oligomer deep cooling trapping system is controlled to reach the oligomer condensation temperature and the liquid phase is discharged, the catalyst starts to initiate the polymerization reaction.
As a preferable scheme of the invention, whether the polymerization catalyst initiates the polymerization reaction is judged by detecting whether the oligomer collecting tank collects liquid-phase substances in the oligomer deep cooling collecting system, and the severity of the polymerization reaction initiated by the polymerization catalyst is judged by detecting the liquid level change rate of the oligomer collecting tank.
As a preferred embodiment of the present invention, the oligomer cryogenic capture system comprises one or more stages of oligomer condensers, one or more stages of droplet coalescers, and an oligomer collection tank. The material flow extracted from the circulating gas of the polymerization reaction system sequentially flows through one-stage or multi-stage oligomer condensers which are connected in series, then flows through one-stage or multi-stage droplet coalescers, liquid-phase oligomers which are liquefied by deep cooling are collected at the bottoms of the oligomer condensers and the droplet coalescers, and the liquid-phase oligomers intensively flow into an oligomer collecting tank for detection.
As a preferable embodiment of the present invention, the outlet temperature of the oligomer condenser is controlled to be-20 ℃ to-30 ℃.
The invention has the beneficial effects that: on the basis of the theory that polymerization and oligomerization of polymerization monomers are simultaneously initiated by a polymerization catalyst, the method monitors the liquid level change of the liquid outlet tank of the oligomer cryogenic capture system by using the existing oligomer cryogenic capture system, can realize the rapid detection and real-time monitoring of the initiation condition of the polymerization reaction at the initial startup of the catalyst polyolefin process, accurately predicts the reaction process, timely adjusts the catalyst addition amount to ensure the startup safety, and prevents the polymerization accidents caused by excessive initiation or the large waste of nitrogen and polymerization monomers caused by no initiation of the catalyst.
Drawings
FIG. 1 is a diagram of a polyolefin production and vent gas recovery process.
FIG. 2 is a flow chart of a reaction process monitored by an oligomer cryogenic capture system during start-up.
The system comprises an X-polymerization reaction system, a Y-oligomer cryogenic trapping system, a circulating gas compressor, a circulating gas cooler, a polymerization reactor, a primary oligomer condenser, a secondary oligomer condenser and a fog droplet coalescer, wherein the X-polymerization reaction system, the Y-oligomer cryogenic trapping system, the circulating gas compressor, the circulating gas cooler, the polymerization reactor, the primary oligomer condenser, the secondary oligomer condenser and the fog droplet coalescer are sequentially connected. 7-oligomer collecting tank, a-polymerization monomer, b-hydrogen, c-recycle gas side line discharging, d-oligomer, e-discharge gas to torch, f-liquid nitrogen feeding, g-liquid nitrogen discharging.
FIG. 3 is a graph showing the correlation between 1-butene in the collected liquid and the concentration of 1-butene in the recycle gas.
Detailed Description
The invention will be further illustrated and described with reference to specific embodiments. The technical features of the embodiments of the present invention can be combined correspondingly without mutual conflict.
As shown in fig. 2, in this embodiment, taking the starting process of a HDPE plant producing 30 ten thousand tons annually by a gas phase method as an example, in a polymerization reaction system, a polymerized monomer a and hydrogen b are pressurized by a compressor 1 and cooled by a cooler 2, and then enter a polyolefin fluidized bed reactor 3 for polymerization reaction, unreacted gas-phase polymerized monomer and hydrogen circularly flow into the compressor 1 from the top of the reactor, and a circulating gas side stream c of 1000kmol/hr flows into an oligomer cryogenic trapping system at a pressure of 20 bar. In the oligomer deep cooling trapping system, a circulating gas side line discharge stream c sequentially enters a two-stage oligomer condenser, the lowest outlet temperature is-28 ℃, and then enters a fog drop coalescer 6 to recover oligomer fog drops in a dispersed gas phase, an oligomer d is enriched in the condenser and the fog drop coalescer, and discharged from the bottom to enter an oligomer collecting tank 7. The remaining gas e is discharged from the top of the mist droplet coalescer 6 into a flare for disposal.
The catalyst used during the start-up of the device is an S-2 type chromium catalyst, a polymerization monomer is introduced at the initial stage, the reaction condition of the reactor 3 is controlled, no catalyst is added, and a liquid phase is not collected by the oligomer collecting tank 7. About 40 minutes after the catalyst is added, the oligomer collecting tank 7 collects the liquid phase, which indicates that the catalyst starts to initiate the polymerization reaction, and as the reaction time increases, the flow of the stream entering the oligomer collecting tank increases, which indicates that the release of the catalyst activity is accelerated and the severity of the polymerization reaction gradually increases. And the content of 1-butene in the recycle gas can be estimated by detecting the content of 1-butene in the collected liquid, and the concentration of 1-butene in the collected liquid and the concentration of 1-butene in the recycle gas have a corresponding relationship shown in figure 3.
The operator can adjust subsequent work in time according to the flow of the oligomer collecting tank, such as the adjustment of parameters of catalyst addition amount, temperature, pressure and the like, and polymerization accidents caused by excessive initiation or a great amount of waste of polymerization monomers caused by no initiation of the catalyst are prevented. During the starting of the chromium catalyst polyolefin process in other industrial devices, an oligomer cryogenic trapping system is adopted to enrich oligomers, whether the chromium catalyst successfully initiates polymerization reaction can be judged according to whether the chromium catalyst is discharged, the oligomer flow is calculated by detecting the liquid level change of an oligomer collecting tank, and the intensity of the polymerization reaction can also be reflected, so that the analysis and judgment method is feasible. The following conclusions can be drawn from the above examples: (1) according to the mechanism that the chromium-based catalyst can catalyze polymerization monomer oligomerization and polymerization of polymerization monomer, the condition that the catalyst initiates polymerization monomer polymerization at the initial starting stage of the process can be judged by adopting the oligomer deep-cooling trapping system to enrich oligomers. This judgment method was found to be accurate and feasible according to a number of applications on devices in the polyolefin industry. (2) According to the device start result, if the liquid phase discharge can be monitored from the oligomer deep cooling trapping system after the catalyst is put into the device for 40 minutes, the chromium-based catalyst can be basically judged to successfully initiate the polymerization reaction of the polymerized monomer, otherwise, the chromium-based catalyst can be predicted not to successfully initiate the polymerization reaction of the polymerized monomer. (3) The concentration of the oligomer in the circulating gas in the reaction system can be reversely deduced according to the effluent flow of the oligomer, so that whether the addition amount of the catalyst is proper or not and whether the intensity of the polymerization reaction is normal or not can be explained, and the method can be used for guiding operators to adjust various parameters.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (3)
1. A method for rapidly judging the driving state of a gas-phase polyolefin production device, wherein the polyolefin is polyethylene, and the method is characterized by comprising the following steps:
leading a stream of circulating gas of a polymerization reaction system out to enter an oligomer deep cooling trapping system, and collecting liquid-phase oligomer after deep cooling; judging whether a polymerization catalyst initiates polymerization reaction or not by detecting whether a liquid phase substance is collected by a oligomer collecting tank in the oligomer deep cooling collecting system or not, and judging the intensity of the polymerization reaction initiated by the polymerization catalyst by detecting the liquid level change rate of the oligomer collecting tank;
the liquid-phase oligomer mainly comprises 1-butene and 1-hexene; the polymerization reaction system adopts a chromium catalyst; the oligomer cryogenic capture system comprises one or more stages of oligomer condensers, one or more stages of droplet coalescers, and an oligomer collection tank; the material flow extracted from the circulating gas of the polymerization reaction system sequentially flows through one-stage or multi-stage oligomer condensers which are connected in series, then flows through one-stage or multi-stage droplet coalescers, liquid-phase oligomers which are liquefied by deep cooling are collected at the bottoms of the oligomer condensers and the droplet coalescers, and the liquid-phase oligomers intensively flow into an oligomer collecting tank for detection.
2. The method for rapidly judging the driving state of a gas-phase polyolefin production device according to claim 1, wherein the outlet temperature of the oligomer condenser is controlled to be-20 ℃ to-30 ℃.
3. The method of rapidly judging the start-up state of a gas phase process polyolefin production plant according to claim 1 wherein the gas phase stream after cryogenic cooling is discharged to flare treatment.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59193128A (en) * | 1983-04-15 | 1984-11-01 | Matsushita Electric Works Ltd | Monitoring system of abnormality in reaction stage |
| CN1732187A (en) * | 2002-12-26 | 2006-02-08 | 尤尼威蒂恩技术有限责任公司 | Static measurement and detection in a gas phase polyethylene reactor |
| EP2059540A1 (en) * | 2006-09-07 | 2009-05-20 | Univation Technologies, LLC | Methods for on-line determination of degree of resin stickiness using a model for depression of melt initiation temperature |
| CN102453153A (en) * | 2010-10-20 | 2012-05-16 | 中国石油化工股份有限公司 | Method for judging polymerization reaction condition at initial production stage of polyethylene process |
| CN103076094A (en) * | 2011-10-26 | 2013-05-01 | 中国石油化工股份有限公司 | Method for detecting reaction state in agitated bed reactor |
-
2021
- 2021-02-04 CN CN202110157376.3A patent/CN112973593B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59193128A (en) * | 1983-04-15 | 1984-11-01 | Matsushita Electric Works Ltd | Monitoring system of abnormality in reaction stage |
| CN1732187A (en) * | 2002-12-26 | 2006-02-08 | 尤尼威蒂恩技术有限责任公司 | Static measurement and detection in a gas phase polyethylene reactor |
| EP2059540A1 (en) * | 2006-09-07 | 2009-05-20 | Univation Technologies, LLC | Methods for on-line determination of degree of resin stickiness using a model for depression of melt initiation temperature |
| CN102453153A (en) * | 2010-10-20 | 2012-05-16 | 中国石油化工股份有限公司 | Method for judging polymerization reaction condition at initial production stage of polyethylene process |
| CN103076094A (en) * | 2011-10-26 | 2013-05-01 | 中国石油化工股份有限公司 | Method for detecting reaction state in agitated bed reactor |
Non-Patent Citations (1)
| Title |
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| 气体液体固体中微量烷烃的分析方法;童清木;《第二次全国石油化工色谱学术报告会文集 上》;19861130;第145-148页 * |
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