CN103091426A - On-line pretreatment device of chromatographic gas sample and application method thereof - Google Patents
On-line pretreatment device of chromatographic gas sample and application method thereof Download PDFInfo
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Abstract
The invention provides an on-line pretreatment device of a chromatographic gas sample, and the device is mainly used for on-line pretreatment of gas samples of an ethylene cracking furnace. The pretreatment device is a box structure, and is mounted between an outlet of an online analysis sampler of the ethylene cracking furnace and an on-line chromatogram. The on-line pretreatment device is mainly composed of a buffer sedimentation tank, a visual liquid-discharge tank, a gas filter, a pressure regulating valve, a cleaning transfer valve, a steam system and insulating parts. Inner surfaces of the connecting pipelines use ultramicro nanostructures with a low surface tension. The chromatographic gas sample can be treated to remove water, solid impurities and heavy hydrocarbon droplets, and outputted to the on-line chromatogram with a stable flow.
Description
Technical field
The present invention relates to a kind of sample processing device for gas chromatographic analysis, more particularly, relate to a kind of pretreatment unit and using method thereof for on-line analysis cracking furnace gas sample.
Background technology
Petrochemical industry is mainstay of the national economy industry, and ethylene unit is the faucet device of petrochemical industry, and the method for ethylene production is a lot, but the most ripe with the pyrolysis in tubular furnace technology, most ethene is all produced by the pyrolysis in tubular furnace method in the world.As the important device in the petrochemical iy produced process, the major control target of ethane cracking furnace is to control the selectivity of cracking severity, turnout and product, and effectively cracking operation depends on the accurate on-line analysis to quencher outlet pyrolysis gas., water cut high due to ethane cracking furnace exported product temperature be large, it is complicated to form, and the demand of controlling according to pyrolysis furnace selects hydrogen, methane, ethene, ethane, propylene, propane as the detected components of on-line analysis usually.On-line chromatograph have measurement range wide, analyze accurately, analytical cycle is short, automaticity is high, analyze that data continuity is strong, data can feed back to the DCS system and be used for the advanced characteristics of controlling, therefore in the industrial ethylene cracker, use on-line chromatograph that key component in pyrolysis gas is analyzed, the parameters such as cracking depth of cracking furnace are monitored and controlled.
because cracking of ethylene outlet of still pyrolysis gas temperature is high, water cut is large, form complicated, comprise hydrogen, methane, ethene, ethane, propylene, the light constituents such as propane, pyrolysis gasoline is also arranged, diesel oil, the viscous component such as tar, also has sour gas etc., its boiling point is from subzero more than 250 degree to several Baidu above freezing, because can causing whole online sampling analytical system, stops up solid impurity, moisture, heavy hydrocarbons etc. can cause the pollution of on-line chromatograph, shorten serviceable life, degradation problem under data accuracy, therefore need to use the pyrolysis gas sampling system to remove solid impurity in the pyrolysis product sample in actual application, moisture and heavy hydrocarbon component, the pyrolysis gas sample is outputed to online gc.
The online gc sampling system that present large and medium-sized ethylene producing device generally uses mainly comprises several parts of sampler, sample pretreatment system and sample operating system.Sampler is generally the whirlpool refrigeratory, be installed on pyrolysis furnace products export process pipeline, the lysate sample of complexity is purified, reflux section and cooled dehydrated section after filtration, solid particle, heavy hydrocarbon component and moisture are back to process pipe, light constituent is exported to sample pretreatment system uniformly with certain flow velocity; The effect of sample pretreatment system is that sample is further purified and exports to sample operating system; Sample operating system is installed on the on-line chromatograph front end, and Main Function comprises stream switching, atmospheric equilibrium and the switching of correction gas circuit.
the pyrolysis furnace on-line analysis system is in actual moving process, cracking on-line analysis sample position is positioned at the pyrolysis furnace products export, sample temperature is high, contain the liquid heavy constituents such as large water gaging and a large amount of tar, owing to inevitably containing liquid component and impurity particle in sample, the sampling process pipeline easily stops up, in addition because there is more problem at present in pretreatment system, it is more that the sample that enters on-line chromatograph contains heavy constituent, cause the pollution of chromatographic column, analyze all problems such as larger of data fluctuations scope and frequency, on-line chromatograph can't be continuous, stable operation, be difficult to provide the basic data of controlling accurately cracking depth of cracking furnace.
Summary of the invention
In order to solve the problem that exists in existing ethane cracking furnace on-line analysis process, the invention provides the online pretreatment unit of a kind of sample gas and using method, the on-line analysis sample that the pyrolysis furnace products export is obtained through the whirlpool refrigeratory is processed.This device need not to former pyrolysis furnace sampling system transformation, be installed and used easy; By removing liquid, the solid impurity in sample, regulate sample flow, export chromatogram to sample gas is clean, stable, realize that the ethane cracking furnace on-line analysis is steady in a long-term, accurately operation.
The online pretreatment unit of a kind of chromatogram gas sample of the present invention is achieved in that
A kind of online pretreatment unit of chromatogram gas sample is entrained with water and heavy hydrocarbon in described chromatogram gas sample;
Described pretreatment unit a4 comprises: casing 11, buffering slurry tank 2, Drainage tank 4, tapping valve 5, gas filter 6, pressure-regulating valve 8 and associated line; Being distributed with on the inside surface of described associated line is highly the tiny projection of 1～100 micron, and this tiny projection is comprised of the ultra tiny minor structure of nanoscale, forms the ultra micro nanostructured of low surface tension; Described chromatogram gas sample enters buffering slurry tank 2 and carries out sedimentation separation by associated line, separates the liquid phase that obtains and enters Drainage tank 4, then discharge described pretreatment unit a4 through tapping valve 5; Separate the gas phase that obtains and enter gas filter 6, then through after pressure-regulating valve 8 adjustings and steady pressure, continuous Input Online chromatogram a5.
During concrete enforcement, described pretreatment unit a4 also comprises: the Steam Heating pipeline 10 and the cabinet insulation layer that are used for heating casing 11.Described pretreatment unit a4 also comprises: be positioned at pressure-regulating valve 8 cleaning transfer valve 9 afterwards, described cleaning transfer valve 9 is T-valve, the steam and the described on-line chromatograph a5 that connect respectively chromatogram gas sample, be used for to clean, when the pipeline pollution between online pretreatment unit a4 and on-line chromatograph a5, obstruction, can cut off the output of chromatogram gas sample, and utilize the described pipeline of steam flush.
The preferred embodiment of the invention is:
Described pretreatment unit a4 comprises: casing 11, buffering slurry tank 2, the visual Drainage tank 4 that can observe liquid level, tapping valve 5, gas filter 6, pressure-regulating valve 8, clean transfer valve 9 after being positioned at pressure-regulating valve 8, the Steam Heating pipeline 10 and the cabinet insulation layer that are used for heating casing 11, and associated line;
Described associated line adopts stainless steel, its inside surface utilizes super hydrophobic coating to process, the height that the ultra tiny minor structure by 50～100 nanometer particle sizes of distributing on this inside surface forms is the tiny projection of 10～20 microns, the ultra micro nanostructured of formation low surface tension;
Described chromatogram gas sample enters buffering slurry tank 2 and carries out sedimentation separation by associated line, separates the liquid phase that obtains and enters Drainage tank 4, then discharge described pretreatment unit a4 through tapping valve 5; Separate the gas phase that obtains and enter gas filter 6, then through after pressure-regulating valve 8 adjustings and steady pressure, continuous Input Online chromatogram a5.
Described cleaning transfer valve 9 is T-valve, connect respectively chromatogram gas sample, clean steam and described on-line chromatograph a5, pipeline between online pretreatment unit a4 and on-line chromatograph a5 pollutes, when stopping up, can cut off the output of chromatogram gas sample, and utilize the described pipeline of steam flush.
The using method of the online pretreatment unit of the present invention is achieved in that
Described chromatogram gas sample is sample gas of ethylene cracking furnace, wherein is entrained with water and heavy hydrocarbon;
use inside surface to be the associated line of the ultra micro nanostructured of low surface tension, the outlet that is installed on the whirlpool refrigeratory of ethane cracking furnace is connected to the buffering slurry tank (2) of described pretreatment unit (a4), the chromatogram gas sample path of described cleaning transfer valve (9) is connected to on-line chromatograph (a5), with the cleaning steam passage of described cleaning transfer valve (9) be connected to Steam Heating pipeline (10) outlet, pyrolysis furnace middle pressure steam recovery line is connected to Steam Heating pipeline (10) import, and to described whirlpool refrigeratory and described on-line chromatograph (a5) and the omnidistance companion's heat of the associated line of described pretreatment unit (a4),
By the next pyrolysis gas sample of the whirlpool refrigeratory of ethane cracking furnace, pass through associated line, the buffering slurry tank 2 that enters described pretreatment unit a4 carries out sedimentation separation, water and the heavy hydrocarbon carried secretly in described pyrolysis gas sample enter Drainage tank 4 after sedimentation separation, discharging described pretreatment unit a4 through tapping valve 5; Separate the gas phase that obtains and enter gas filter 6, then through after pressure-regulating valve 8 adjustings and steady pressure, the sample operating system of continuous Input Online chromatogram a5 leading portion also finally enters on-line chromatograph a5;
When described pretreatment unit a4 operation, utilize described Steam Heating pipeline 10 heating casings 11, utilize described cabinet insulation layer insulation;
When the pipeline between online pretreatment unit a4 and on-line chromatograph a5 pollutes, when stopping up, switches and clean transfer valve 9 cut-out chromatogram gas sample outputs, utilize middle pressure steam to rinse above-mentioned pipeline.
The online pretreatment unit of sample gas of ethylene cracking furnace is mounted in the box unit of ethane cracking furnace on-line analysis sampler outlet, the entrance of pretreatment unit is connected with the whirlpool cooler outlet by the stainless steel pipeline, and the pretreatment unit outlet is connected to the sample operating system of line chromatogram leading portion and finally enters on-line chromatograph by the stainless steel pipeline
At first the pyrolysis gas sample of whirlpool refrigeratory output enters the buffering slurry tank, the water of carrying secretly and heavy hydrocarbon be sedimentation and final by visual Drainage tank discharge in tank, gaseous sample further purifies by gas filter, then carries out pressure by tensimeter and pressure-regulating valve and regulate with stable flow output.
This device feature uses the stainless steel pipeline to connect, connect with stainless steel pipeline inside surface all through processing, adopt the ultra micro nanostructured of low surface tension: inner surface of pipeline distribution tiny projection (1～100 micron), each projection is comprised of the ultra tiny kick of nanoscale again.Due to the part of the depression between each projection gassy, be close on wall form one deck as thin as a wafer, only have the thick gas blanket of nanoscale, when drop is attached to wall like this, due on size much larger than this structure, drop and wall main body can only be with the protruding point contacts of the several microspikes of wall across one deck air as thin as a wafer.Drop forms under the surface tension effects of self or near spherical, causes the effect of similar " lotus leaf effect ".Drop more easily rolls, landing, enter fluid collection device under gravity or gas purging, avoided causing following result: the residual wall that is attached to of liquid phase, may carry liquid phase impurity secretly in the gas flow process, thereby liquid phase enters chromatographic column with gaseous sample pollutes chromatograph, causes on-line analysis system to work.
Take Steam Heating in this device box, the middle pressure steam of ethylene unit enters by a switch valve and returns to vapour line after tubulation in casing heats casing.Covering insulation material in device box.Pollute, when stopping up, can cut off the output of chromatogram gas sample, and utilize the described pipeline of steam flush when the online pretreatment unit of sample gas to the pipeline between on-line chromatograph three-way switch valve is installed after pressure-regulating valve.
Outstanding feature of the present invention is: (1) need not be to former pyrolysis furnace sampling system transformation, simple installation, and working stability is reliable, not affected by changes in environmental conditions.(2) this device adopts integrated form design easy to use and safeguard.(3) this device effectively purifies and voltage stabilizing pyrolysis furnace on-line analysis sample, be conducive to the stable of gas composition, the inside surface of associated line adopts the ultra micro nanostructured of low surface tension, drop can effectively be eliminated resident, for on-line chromatograph provides stable, clean analytic sample gas, thereby guarantee the permanently effective operation of on-line chromatograph energy, analyze data accurate, stable, can realize cracking severity control for pyrolysis furnace provides data basic.
Description of drawings
Fig. 1: the online pretreatment unit schematic diagram of sample gas of ethylene cracking furnace;
Fig. 2: ethane cracking furnace on-line analysis Logistics Process schematic diagram
Embodiment
The below contrasts accompanying drawing, is described in further detail technical scheme of the present invention in conjunction with the embodiments, and protection scope of the present invention is not limited to following embodiment.
(1) pretreatment unit of sample gas of ethylene cracking furnace on-line chromatograph analysis:
Be entrained with water and heavy hydrocarbon in sample gas of ethylene cracking furnace; This pretreatment unit comprises: casing 11, buffering slurry tank 2, the visual Drainage tank 4 that can observe liquid level, tapping valve 5, gas filter 6, pressure-regulating valve 8, clean transfer valve 9 after being positioned at pressure-regulating valve 8, the Steam Heating pipeline 10 and the cabinet insulation layer that are used for heating casing 11, and associated line; The associated line of this pretreatment unit adopts stainless steel, and its inside surface utilizes super hydrophobic coating to process, and forms the ultra micro nanostructured of low surface tension, the tiny projection of 10 microns left and right that the ultrastructure about wall distribution 100 nanometers forms; Cleaning transfer valve 9 is T-valve, connects respectively chromatogram gas sample, cleans steam and described on-line chromatograph a5.
(2) using method of the pretreatment unit of sample gas of ethylene cracking furnace on-line chromatograph analysis:
(1) connected mode of this device is:
The outlet that is installed on the whirlpool refrigeratory of ethane cracking furnace is connected to the buffering slurry tank 2 of described pretreatment unit, the chromatogram gas sample path that cleans transfer valve 9 is connected to on-line chromatograph a5, the cleaning steam passage of described transfer valve 9 is connected to middle pressure steam, and to the omnidistance companion's heat of the associated line of described whirlpool refrigeratory and described on-line chromatograph a5 and described pretreatment unit;
By the next pyrolysis gas sample of the whirlpool refrigeratory of ethane cracking furnace, pass through associated line, enter buffering slurry tank 2 and carry out sedimentation separation, the water of carrying secretly in the pyrolysis gas sample and heavy hydrocarbon enter Drainage tank 4 after sedimentation separation, are discharging pretreatment unit through tapping valve 5; Separate the gas phase that obtains and enter gas filter 6, then through after pressure-regulating valve 8 adjustings and steady pressure, the sample operating system of continuous Input Online chromatogram a5 leading portion also finally enters on-line chromatograph a5;
When pretreatment unit moves, utilize described Steam Heating pipeline 10 heating casings 11, utilize described cabinet insulation layer insulation; When the pipeline between online pretreatment unit and on-line chromatograph a5 pollutes, when stopping up, switches and clean transfer valve 9 cut-out chromatogram gas sample outputs, utilize middle pressure steam to rinse above-mentioned pipeline.
In use but the whirlpool refrigeratory of one or more ethane cracking furnace shares 1 on-line chromatograph a5 by pipeline.The cracking on-line sample is taken out from pyrolysis furnace outlet process pipeline a1, arrives on-line chromatograph a5 and analyzes by whirlpool refrigeratory a2, the online pre-service a4 of sample gas of ethylene cracking furnace, sample operating system a4 successively.
(2) mode of operation of this device is:
confirm that pyrolysis furnace whirlpool refrigeratory is in closed condition, after finishing device is installed, all switch valve is in closed condition, confirm that three-way switch valve 9 is in the B position, open switch valve 10, middle pressure steam 12 enters the heating pipeline device is heated, after stablizing 10 minutes, open switch valve 1 and open pyrolysis furnace whirlpool refrigeratory, sample gas 11 enters the online pretreatment unit of sample gas of ethylene cracking furnace successively by hydrops tank 2, gas filter 6, tensimeter 7, pressure-regulating valve 8, three-way switch valve 9, adjusting pressure-regulating valve 8 is observed simultaneously tensimeter 7 sample strain is adjusted to 80～100KPa, sample through purifying also finally arrives on-line chromatograph a5 with stable flow to follow-up pipeline output.
(3) this device is patrolled and examined, maintenance mode is:
In the situation of ethane cracking furnace smooth operation, patrol and examine every day and determine that tensimeter 7 readings are normal, using infrared thermometer determinator inner part appearance temperature is 50～60 ℃; Carry out weekly a discharge opeing, open switch valve 3 and make the liquid in hydrops tank 2 flow into visual Drainage tank 4, then shut-off valve 3 is opened switch valve 5 and is carried out discharge opeing; Check per month gas filter 6, according to circumstances carry out filter element replacing.
When the online pretreatment unit of sample gas to the pipeline between on-line chromatograph a5 pollutes, when stopping up, can cut off sample gas output by switch three-way valve 9, open simultaneously valve 12 and use the middle pressure steam clean-up line.
By steam insulation, keep temperature stabilization in casing, reduce hydrocarbon component because temperature variation is condensed; Device is obvious to the water in sample gas, solid particle and heavy hydrocarbon drop filter effect; The pipeline inside surface adopts the ultra micro nanostructured of low surface tension, has avoided the liquid phase wall built-up, effectively eliminates sampling line, on-line chromatograph latch up phenomenon, has avoided carrying fine droplet in gaseous sample secretly, has avoided chromatographic column contaminated and analyze the situation of data fluctuations; Set the online pretreatment unit pressure of sample gas and be controlled to be 80～100Kpa, sample flow is stablized controlled, has avoided flow rate fluctuation on-line chromatograph to be analyzed the impact of data; The situation that sample condenses in pipeline is eliminated substantially.By this device, make that the gaseous sample that enters chromatogram is stable, cleaning, analysis result can truly reflect the real time execution situation of pyrolysis furnace, for the Real-Time Monitoring of cracking, control data supporting is provided, can effectively improve the advanced control level of pyrolysis furnace.
Claims (5)
1. the online pretreatment unit of a chromatogram gas sample, be entrained with water and heavy hydrocarbon in described chromatogram gas sample;
Described pretreatment unit (a4) comprising: casing (11), buffering slurry tank (2), Drainage tank (4), tapping valve (5), gas filter (6), pressure-regulating valve (8) and associated line;
Being distributed with on the inside surface of described associated line is highly the tiny projection of 1～100 micron, and this tiny projection is comprised of the ultra tiny minor structure of nanoscale, forms the ultra micro nanostructured of low surface tension;
Described chromatogram gas sample enters buffering slurry tank (2) and carries out sedimentation separation by associated line, separates the liquid phase that obtains and enters Drainage tank (4), then pass through tapping valve (5) and discharge described pretreatment unit (a4); Separate the gas phase that obtains and enter gas filter (6), then after passing through pressure-regulating valve (8) adjusting and steady pressure, continuous Input Online chromatogram (a5).
2. online pretreatment unit according to claim 1 is characterized in that:
Described pretreatment unit (a4) also comprises: the Steam Heating pipeline (10) and the cabinet insulation layer that are used for heating casing (11).
3. online pretreatment unit according to claim 1 is characterized in that:
Described pretreatment unit (a4) also comprises: be positioned at pressure-regulating valve (8) cleaning transfer valve (9) afterwards, described cleaning transfer valve (9) is T-valve, the steam and the described on-line chromatograph (a5) that connect respectively chromatogram gas sample, be used for to clean, when the pipeline pollution between online pretreatment unit (a4) and on-line chromatograph (a5), obstruction, can cut off the output of chromatogram gas sample, and utilize the described pipeline of steam flush.
4. online pretreatment unit according to claim 1 is characterized in that:
Described pretreatment unit (a4) comprising: casing (11), buffering slurry tank (2), the visual Drainage tank (4) that can observe liquid level, tapping valve (5), gas filter (6), pressure-regulating valve (8), be positioned at pressure-regulating valve (8) and clean afterwards transfer valve (9), the Steam Heating pipeline (10) and the cabinet insulation layer that are used for heating casing (11), and associated line;
Described associated line adopts stainless steel, its inside surface utilizes super hydrophobic coating to process, the height that the ultra tiny minor structure by 50～100 nanometer particle sizes of distributing on this inside surface forms is the tiny projection of 10～20 microns, the ultra micro nanostructured of formation low surface tension;
Described chromatogram gas sample enters buffering slurry tank (2) and carries out sedimentation separation by associated line, separates the liquid phase that obtains and enters Drainage tank (4), then pass through tapping valve (5) and discharge described pretreatment unit (a4); Separate the gas phase that obtains and enter gas filter (6), then after passing through pressure-regulating valve (8) adjusting and steady pressure, continuous Input Online chromatogram (a5).
Described cleaning transfer valve (9) is T-valve, connect respectively chromatogram gas sample, clean steam and described on-line chromatograph (a5), when the pipeline pollution between online pretreatment unit (a4) and on-line chromatograph (a5), obstruction, can cut off the output of chromatogram gas sample, and utilize the described pipeline of steam flush.
5. the using method of online pretreatment unit according to claim 4:
Described chromatogram gas sample is sample gas of ethylene cracking furnace, wherein is entrained with water and heavy hydrocarbon;
use inside surface to be the associated line of the ultra micro nanostructured of low surface tension, the outlet that is installed on the whirlpool refrigeratory of ethane cracking furnace is connected to the buffering slurry tank (2) of described pretreatment unit (a4), the chromatogram gas sample path of described cleaning transfer valve (9) is connected to on-line chromatograph (a5), with the cleaning steam passage of described cleaning transfer valve (9) be connected to Steam Heating pipeline (10) outlet, pyrolysis furnace middle pressure steam recovery line is connected to Steam Heating pipeline (10) import, and to described whirlpool refrigeratory and described on-line chromatograph (a5) and the omnidistance companion's heat of the associated line of described pretreatment unit (a4),
By the next pyrolysis gas sample of the whirlpool refrigeratory of ethane cracking furnace, pass through associated line, the buffering slurry tank (2) that enters described pretreatment unit (a4) carries out sedimentation separation, the water of carrying secretly in described pyrolysis gas sample and heavy hydrocarbon enter Drainage tank (4) after sedimentation separation, discharging described pretreatment unit (a4) through tapping valve (5); Separate the gas phase that obtains and enter gas filter (6), then after passing through pressure-regulating valve (8) adjusting and steady pressure, the sample operating system of Input Online chromatogram (a5) leading portion also finally enters on-line chromatograph (a5) continuously;
When described pretreatment unit (a4) moves, utilize described Steam Heating pipeline (10) heating casing (11), utilize described cabinet insulation layer insulation;
When the pipeline between online pretreatment unit (a4) and on-line chromatograph (a5) pollutes, when stopping up, switches and clean the output of transfer valve (9) cut-out chromatogram gas sample, utilize middle pressure steam to rinse above-mentioned pipeline.
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| CN112725039A (en) * | 2020-12-21 | 2021-04-30 | 西安鼎研科技股份有限公司 | System and method for analyzing CO concentration of nitrogen blow-down pipe of nozzle cooling separator of coal gasification furnace |
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