CN106554790A - The separation method of the liquid product obtained in ethane cracking furnace calibration process - Google Patents
The separation method of the liquid product obtained in ethane cracking furnace calibration process Download PDFInfo
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Abstract
The present invention relates to a kind of separation method, and in particular to a kind of separation method of the liquid product obtained in ethane cracking furnace calibration process.The liquid product obtained in ethane cracking furnace calibration process is carried out into standing sedimentation, liquid product is divided into three-phase, respectively tar phase, Emulsion Phase and water phase;Flocculant will be added after three phase separation in Emulsion Phase, while ultrasound is carried out, sub-argument water outlet phase and tar phase after standing.Instant invention overcomes the current deficiency of tar water separating process, by ultrasound wave and flocculant group technology, being kept completely separate for water and tar is realized, it is ensured that the accuracy of sample analysis in calibration process, to determine the optimal cracking technology condition of pyrolysis furnace.
Description
Technical field
The present invention relates to a kind of separation method, and in particular to a kind of separation of the liquid product obtained in ethane cracking furnace calibration process
Method.
Background technology
Steam cracking refer to petroleum hydrocarbon occur under conditions of high temperature (more than >=750 DEG C) and vapor are present molecular breakdown and
Dehydrogenation reaction, with the process of the reactions such as a small amount of polymerization, condensation.Steam cracking is the low-molecular olefines such as production ethylene, propylene
Main method, is the basis of powerful petro chemical industry.
The main purpose of industrial steam cracker is preparing ethylene.At present, 98% ethylene source is filled in steam cracking in the world
Put.While ethylene is produced, the industrial steam cracker also low-molecular olefine such as by-product propylene, butadiene, and benzene, first
The light aromatics such as benzene, dimethylbenzene, also generate a small amount of heavy arene in addition.
One complete steam cracking process includes cracking, chilling, compression and separates four operations.Cracking refers to steam cracking
Reaction, cracking stock and dilution steam generation are reached across section temperature, then into radiant section through preheating section according to certain ratio,
Cracking reaction is carried out, steam cracking is the endothermic reaction, generally carried out in tubular heater.Chilling is generally referred to pyrolysis furnace
Quenching boiler (TLE) exports 450 DEG C or so of Pintsch process air cooling to 40 DEG C, sub-department's Pyrolysis fuel oil PFO, pyrolysis gas oil,
Drippolene and fresh water (FW), and cracking gas is sent into into one section of entrance of compressor.The chilling stage, existing heat transfer had dividing for material again
From.Compressibility mainly includes cracking gas compression, abjection sour gas and drying and chilling.By compression, on the one hand can carry
The detached operation temperature of high deep cooling, so as to save cryogenic energy and cryogenic material;On the other hand pressurization can promote in cracking gas water and
Heavy hydrocarbon is condensed, so considerable amount of moisture and heavy hydrocarbon can be removed, so as to reduce drying and dehydrating and the detached burden of rectification.
In piece-rate system, acetylene and propine will be removed by hydrogenation, while methane is converted carbon monoxide to, then by heat exchange and essence
Fraction is from the separation for realizing ethylene, propylene, carbon four, ethane, methane, propane etc..
Cracking technology condition is referred in the case where the pyrolysis furnace type of furnace is certain, and cracking temperature, thinner ratio, the time of staying, pyrolysis furnace go out
Mouth pressure and some other adjustable parameters.By the adjustment of process conditions, pyrolysis product maximizing the benefits is made.Steam
The raw material range of cracking is very wide, and the petroleum distillate up to 560 DEG C from ethane to boiling point can be used as tube cracking furnace cracking ethylene preparation
Raw material.The corresponding optimal cracking technology condition of different cracking stocks is also not quite similar.Under identical raw material, different pyrolysis furnaces
The corresponding optimum cracking technology condition of type is also not quite similar.Under the identical type of furnace and cracking stock, in pyrolysis furnace cycle of operation
Different phase, Optimal technique process are also not quite similar.
To be adjusted to pyrolysis furnace operation process condition in time, to ensure the maximizing the benefits of cracking stock, while dropping as far as possible
Low plant energy consumption, needs to carry out staking-out work to pyrolysis furnace.Calibrating cracking furnace refers in the case where cracking stock is constant, maintains one
Fixed inlet amount, collects the gas-phase product and liquid product under corresponding cracking temperature within a certain period of time;According to same step,
Change cracking temperature, collect gas-phase product and liquid product under relevant temperature.Gas phase under the different temperatures obtained by collection is produced
Thing and liquid product carry out composition analysis using chromatograph, obtain the yield of cracked product under different cracking temperatures, by product yield
Contrast draws the cracking temperature of optimum.
Carrying out when calibrating cracking furnace works, obtaining the mixture that liquid product is water and tar, the presence of emulsion so that nothing
Method accurately obtains the quality of water and tar, and then impact analysis result, ultimately results in yield of cracked product and analyzes inaccurate, causes
The optimal cracking temperature for obtaining non-optimal cracking temperature.Therefore, accurate analysis meter measures tar and the quality of water is split to determination
Solution stove optimum process condition it is critical that.
Patent CN200958057Y discloses a kind of recycle device of oil-containing phenol wastewater in coke tar recovery system.The patent
Mainly include cleaner unit, waste water collector, water tank, pump, ultrasonic emulsator, emulsifying oil tank etc..The patent utilization shallow-layer is managed
By the recycling for realizing oil-containing phenol wastewater.But the device is more complicated, and suitable for the separation process of coal tar.Specially
Sharp CN201410416670 discloses a kind of gas liquor tar separation method.Gas liquor is passed through in ultrasonic container, coal gas is made
Water is sufficiently mixed installed in the coke granule in the separate bed in ultrasonic container with lifting, then applies 30~100kHz of frequency, work(
Rate is the ultrasound wave of 300~1000W, and vibration 30s~15min carries out the coal-tar middle oil detached process of gas liquor, then again by right
Coke granule in separate bed carries out solid-liquid two-phase laminated flow, obtains tar.Wherein described solid/liquid separation can using centrifugation, filter or
Flocculation mode.The technique is realized solid phase, tar and is separated with water three, but the separating effect of tar and water is poor.Patent
CN201110168688 discloses a kind of application of ultrasound wave in biomass tar dehydration.In relatively low temperature environment, utilize
Penetrate and the cavitation effect etc. of ultrasound wave is acted on, and breaks milkiness liquid status of the water in tar, make moisture in biomass coke tar and
Organic principle is layered, and then stands refrigerated separation, removing water and tar.The technique realizes the separation of tar and water, but by
In causing separating effect poor only with single ultrasonic dehydration technology.
It is one of important separation method in current water technology that flocculating sedimentation (or floating on) carries out the method for solid-liquid separation.Using
When aqueous solution high polymer processes industrial wastewater, sanitary wastewater, industrial water supply, recirculated cooling water, domestic use of water for flocculant, tool
There is promotion water quality clarification, accelerate the rate of filtration of settled sludge, reduce body refuse quantity and filter cake is easy to the advantages of disposing.
Flocculant is divided into inorganic flocculating agent and organic flocculant.Inorganic flocculating agent is mainly condensed by the electric charge on neutralization particle,
Therefore commonly referred to as flocculating agent.Conventional inorganic flocculating agent is broadly divided into three classes, and be mainly polymerized Al-based goagulants, polysilicate
Class flocculant and boron mud composite flocculant.Organic flocculant relies primarily on bridging action and makes particle precipitation, therefore and organic-flocculation
Agent is called flocculant or flocculation aid.Organic flocculant can be divided three classes, mainly Syn-Organic flocculants, natural organic
Macromolecule modified flocculant, microbial flocculant.
In view of above-mentioned analysis, separation coal-tar middle oil to calibration process and water is most important.
The content of the invention
For the deficiencies in the prior art, it is an object of the invention to provide the liquid product obtained in a kind of ethane cracking furnace calibration process
Separation method, overcome the deficiency of current tar water separating process, realize being kept completely separate for water and tar, it is ensured that calibration process
The accuracy of middle sample analysis, to determine the optimal cracking technology condition of pyrolysis furnace.
The separation method of the liquid product obtained in ethane cracking furnace calibration process of the present invention, ethane cracking furnace is calibrated
The liquid product obtained in journey carries out standing sedimentation, and liquid product is divided into three-phase, respectively tar phase, Emulsion Phase and water phase;Will
Flocculant is added after three phase separation in Emulsion Phase, while ultrasound is carried out, sub-argument water outlet phase and tar phase after standing.
Wherein:
The liquid product obtained in ethane cracking furnace calibration process is the mixture of tar and water.By in ethane cracking furnace calibration process
The liquid product of acquirement carries out standing sedimentation, and liquid product is divided into three-phase, respectively tar phase, Emulsion Phase and water phase, tar phase
Positioned at upper strata, water is mutually located at lower floor, and Emulsion Phase is located at intermediate layer.
The standing sedimentation time is 0.3h~3h, and the preferred standing sedimentation time is 1h~2h.
When being demarcated in the lab, standing sedimentation used can be separatory funnel, beaker or wide mouthed bottle etc..It is preferred to stand
Settlement instrument is separatory funnel.
Sub-argument water outlet phase and tar phase after standing, wherein time of repose are 0.05h~0.5h, preferred 0.05h~0.2h.
Ultrasound is to carry out ultrasound using supersonic generator, and ultrasonic time is 0.1-0.5h.
Described flocculant is organic flocculant, can be organic polymer coargulator, natural organic high-molecular flocculant or micro- life
Thing flocculant, preferably organic polymer coargulator;
Organic polymer coargulator be primafloc, quaternary ammonium type flocculant or separan, preferably poly- third
Acrylamide type flocculant;Polyacrylamide flocculant is non-ionic flocculant, Flokal B, cationic flocculant or both sexes
Separan, preferably amphiprotic polyacrylamide type flocculant, flocculant are commercially available prod.
The addition of amphiprotic polyacrylamide type flocculant for Emulsion Phase quality 10%~90%.
During with ethane, propane and lighter hydrocarbons as cracking stock, the addition of amphiprotic polyacrylamide type flocculant is Emulsion Phase quality
10%~40%, preferably 15%~25%;During with Petroleum as cracking stock, the addition of amphiprotic polyacrylamide type flocculant is
The 30%~60% of Emulsion Phase quality, preferably 40%~48%;During with tail oil as cracking stock, the flocculation of amphiprotic polyacrylamide type
The addition of agent for Emulsion Phase quality 30%~60%, preferably 50%~60%.
Flocculant is added in Emulsion Phase, while ultrasound is carried out using supersonic generator, to ensure that flocculant is more had
Machine is mutually adsorbed onto in flocculant, and Emulsion Phase is divided into water phase and tar phase.
In sum, the present invention has advantages below:
Instant invention overcomes the deficiency of current tar water separating process, by ultrasound wave and flocculant group technology, realizes water and Jiao
Oily is kept completely separate, it is ensured that the accuracy of sample analysis in calibration process, to determine the optimal cracking technology condition of pyrolysis furnace.
In the water phase obtained after processed by the invention, the content of content water in more than 92wt%, tar phase of water is in below 6wt%.
Specific embodiment
With reference to embodiment, the present invention will be further described.
Embodiment 1
In the calibration process of light hydrocarbon cracking stove, the total 3.5kg of liquid product of acquirement, after standing sedimentation 1.5h, obtains tar
Phase 0.3kg, water phase 2.9kg, Emulsion Phase 0.3kg.0.10kg primaflocs, ultrasound wave are added in the Emulsion Phase for obtaining
0.2h is vibrated, then standing sedimentation 5 minutes.The water for obtaining is mutually 0.18kg, then the tar for obtaining is 0.09kg.It is total to obtain
Water mutually be 3.08kg, tar is 0.39kg.The water phase and tar phase that obtain is determined Jing after the process of embodiment 1 with moisture test apparatus
The content of middle water, as a result respectively 94wt% and 6wt%.
Embodiment 2
In the calibration process of naphtha pyrolysis stove, the total 5.5kg of liquid product of acquirement, after standing sedimentation 1.9h, obtains Jiao
Oil phase 1.2kg, water phase 3.7kg, Emulsion Phase 0.6kg.0.36kg quaternary ammonium type flocculant, ultrasound are added in the Emulsion Phase for obtaining
Ripple vibrates 0.3h, then standing sedimentation 8 minutes.The water for obtaining is mutually 0.4kg, then the tar for obtaining is 0.2kg.It is total to obtain
Water mutually be 4.1kg, tar is 1.4kg.Determined Jing after the process of embodiment 2 in the water phase and tar phase that obtain with moisture test apparatus
The content of water, as a result respectively 92wt% and 5wt%.
Embodiment 3
In the calibration process of tail oil pyrolysis furnace, the total 7.5kg of liquid product of acquirement, after standing sedimentation 2h, obtains tar phase
2.05kg, water phase 4.7kg, Emulsion Phase 0.75kg.0.45kg anion-polyacrylamides wadding is added in the Emulsion Phase for obtaining
Solidifying agent, supersonic oscillations 0.4h, then standing sedimentation 8 minutes.The water for obtaining is mutually 0.46kg, then the tar for obtaining is 0.29kg.
Total water for obtaining is mutually 5.16kg, and tar is 2.34kg.The water phase for obtaining is determined Jing after the process of embodiment 3 with moisture test apparatus
With the content of water in tar phase, as a result respectively 95wt% and 4wt%.
Embodiment 4
In the calibration process of light hydrocarbon cracking stove, the total 3.5kg of liquid product of acquirement, after standing sedimentation 2h, obtains tar phase
0.35kg, water phase 2.98kg, Emulsion Phase 0.17kg.0.4kg cationic-type polyacrylamides wadding is added in the Emulsion Phase for obtaining
Solidifying agent, supersonic oscillations 0.1h, then standing sedimentation 5 minutes.The water for obtaining is mutually 0.13kg, then the tar for obtaining is 0.0.04kg.
Total water for obtaining is mutually 3.11kg, and tar is 0.39kg.The water phase for obtaining is determined Jing after the process of embodiment 4 with moisture test apparatus
With the content of water in tar phase, as a result respectively 94wt% and 4wt%.
Embodiment 5
In the calibration process of naphtha pyrolysis stove, the total 5.5kg of liquid product of acquirement, after standing sedimentation 1.9h, obtains Jiao
Oil phase 1.2kg, water phase 3.7kg, Emulsion Phase 0.6kg.The flocculation of 0.3kg amphiprotic polyacrylamides is added in the Emulsion Phase for obtaining
Agent, supersonic oscillations 0.3h, then standing sedimentation 8 minutes.The water for obtaining is mutually 0.46kg, then the tar for obtaining is 0.14kg.
Total water for obtaining is mutually 4.16kg, and tar is 1.34kg.The water phase for obtaining is determined Jing after the process of embodiment 5 with moisture test apparatus
With the content of water in tar phase, as a result respectively 99wt% and 1wt%.
Embodiment 6
In the calibration process of tail oil pyrolysis furnace, the total 7.5kg of liquid product of acquirement, after standing sedimentation 1.5h, obtains tar
Phase 1.75kg, water phase 4.7kg, Emulsion Phase 1.05kg.The flocculation of 0.45kg amphiprotic polyacrylamides is added in the Emulsion Phase for obtaining
Agent, supersonic oscillations 0.3h, then standing sedimentation 5 minutes.The water for obtaining is mutually 0.76kg, then the tar for obtaining is 0.29kg.
Total water for obtaining is mutually 5.46kg, and tar is 2.04kg.The water phase for obtaining is determined Jing after the process of embodiment 6 with moisture test apparatus
With the content of water in tar phase, as a result respectively 99.5wt% and 0.4wt%.
Claims (10)
1. a kind of separation method of the liquid product for obtaining in ethane cracking furnace calibration process, it is characterised in that:By ethane cracking furnace
The liquid product obtained in calibration process carries out standing sedimentation, and liquid product is divided into three-phase, respectively tar phase, Emulsion Phase and water
Phase;Flocculant will be added after three phase separation in Emulsion Phase, while ultrasound is carried out, sub-argument water outlet phase and tar phase after standing.
2. the separation method of the liquid product for obtaining in ethane cracking furnace calibration process according to claim 1, its feature exist
In:The standing sedimentation time is 0.3h~3h.
3. the separation method of the liquid product for obtaining in ethane cracking furnace calibration process according to claim 1, its feature exist
In:Sub-argument water outlet phase and tar phase after standing, wherein time of repose are 0.05h~0.5h.
4. the separation method of the liquid product for obtaining in ethane cracking furnace calibration process according to claim 1, its feature exist
In:Ultrasound is to carry out ultrasound using supersonic generator, and ultrasonic time is 0.1-0.5h.
5. the separation method of the liquid product for obtaining in ethane cracking furnace calibration process according to claim 1, its feature exist
In:Flocculant is organic flocculant.
6. the separation method of the liquid product for obtaining in ethane cracking furnace calibration process according to claim 5, its feature exist
In:Organic flocculant is primafloc, quaternary ammonium type flocculant or separan.
7. the separation method of the liquid product for obtaining in ethane cracking furnace calibration process according to claim 6, its feature exist
In:Separan is non-ionic flocculant, Flokal B, cationic flocculant or amphiprotic polyacrylamide
Type flocculant.
8. the separation method of the liquid product for obtaining in ethane cracking furnace calibration process according to claim 1, its feature exist
In:Flocculant is amphiprotic polyacrylamide type flocculant.
9. the separation method according to the liquid product obtained in the arbitrary described ethane cracking furnace calibration process of claim 1-8, its
It is characterised by:The addition of amphiprotic polyacrylamide type flocculant for Emulsion Phase quality 10%~90%.
10. the separation method of the liquid product for obtaining in ethane cracking furnace calibration process according to claim 9, its feature
It is:During with ethane, propane and lighter hydrocarbons as cracking stock, the addition of amphiprotic polyacrylamide type flocculant is Emulsion Phase quality
10%~40%;During with Petroleum as cracking stock, the addition of amphiprotic polyacrylamide type flocculant is Emulsion Phase quality
30%~60%;During with tail oil as cracking stock, the addition of amphiprotic polyacrylamide type flocculant for Emulsion Phase quality 30%~
60%.
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JPH0810509A (en) * | 1994-06-30 | 1996-01-16 | Mitsubishi Kakoki Kaisha Ltd | Vessel waste oil treatment |
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CN102288512A (en) * | 2010-06-18 | 2011-12-21 | 中国石油化工股份有限公司 | Method for calibrating yield of cracked product of cracking furnace in ethylene device |
CA2759359A1 (en) * | 2010-12-09 | 2012-06-09 | General Electric Company | Ultra-sound enhanced centrifugal separation of oil from oily solids in water and wastewater |
CN203976443U (en) * | 2014-06-24 | 2014-12-03 | 上海尚江石油工程设备有限公司 | A kind of ultrasonic wave flocculation-air floating device for oily water separation |
CN104556513A (en) * | 2013-10-15 | 2015-04-29 | 中国石油化工股份有限公司 | Sump oil dehydration technology and device |
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2015
- 2015-09-30 CN CN201510641861.2A patent/CN106554790A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH0810509A (en) * | 1994-06-30 | 1996-01-16 | Mitsubishi Kakoki Kaisha Ltd | Vessel waste oil treatment |
CN1803654A (en) * | 2005-12-08 | 2006-07-19 | 南京工业大学 | Oil-containing dross dehydration process |
CN102288512A (en) * | 2010-06-18 | 2011-12-21 | 中国石油化工股份有限公司 | Method for calibrating yield of cracked product of cracking furnace in ethylene device |
CA2759359A1 (en) * | 2010-12-09 | 2012-06-09 | General Electric Company | Ultra-sound enhanced centrifugal separation of oil from oily solids in water and wastewater |
CN104556513A (en) * | 2013-10-15 | 2015-04-29 | 中国石油化工股份有限公司 | Sump oil dehydration technology and device |
CN203976443U (en) * | 2014-06-24 | 2014-12-03 | 上海尚江石油工程设备有限公司 | A kind of ultrasonic wave flocculation-air floating device for oily water separation |
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