CN101747927B - Coke inhibitor for ethylene cracking - Google Patents
Coke inhibitor for ethylene cracking Download PDFInfo
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- CN101747927B CN101747927B CN2009102641926A CN200910264192A CN101747927B CN 101747927 B CN101747927 B CN 101747927B CN 2009102641926 A CN2009102641926 A CN 2009102641926A CN 200910264192 A CN200910264192 A CN 200910264192A CN 101747927 B CN101747927 B CN 101747927B
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Abstract
The invention relates to coke inhibitor for ethylene cracking, which comprises the following component by weight percentage: 20% to 60% of sulfur-containing compound, 5% to 10% of passivator, 1% to 10% of film-forming agent, 5% to 15% of polymerization inhibitor, 1% to 10% of decoking agent and 25% to 45% of solvent, wherein the sulfur-containing compound is particularly dialkyl disulfide, dialkyl sulfide, di-alkylphenol sulfide, diphenyl sulfide, diphenyl disulfide, thiophene or thioxene; and the passivator is particularly triphenyl phosphate, triethyl phosphate, di-octyl-phenyl-phosphate, tributyl phosphate, thiophosphate trilaurate, diethyl-phosphorodi-thioate or triacyl piperidine phosphate, and the passivator is preferably triphenyl phosphate or di-octyl-phenyl-phosphate. The coke inhibitor of the invention for ethylene cracking is capable of effectively relieving the coking condition of an ethylene cracking tube, ensuring the good coke-inhibiting effect, obviously increasing the operation cycle of cracking and reducing the air-decoking time. Therefore, the coke inhibitor of the invention has wide applicable range in the coke inhibition of gaseous light dydrocarbon and naphtha.
Description
Technical field
The present invention relates to a kind of coke inhibitor for ethylene cracking that is used for ethylene cracking tube, belong to oil refining auxiliary agent field.
Background technology
Produce with the hydrocarbon raw material cracking in the method for ethene, the tube furnace steam splitting process accounts for more than 90%.The hydro carbons high temperature pyrolysis unavoidably has by-product coke to generate, and gathers coking dirt layer at the boiler tube inwall, influences furnace tube heat transfer; Energy consumption increases (pyrolyzer account for ethylene production energy consumption 60%), and system pressure rises, so that blocking pipe; Want regular coke cleaning for this reason, comprise that short-period steam-air burns and macrocyclic machinery or hydraulic decoking, frequent clear, burn and not only reduce working rate; Falling 2～10% does not wait; Make boiler tube receive machinery or thermal stresses again, produce creep cavity or crackle, shorten the pyrolyzer life-span.
In the face of an inevitable coking difficult problem, the various countries giant manufacturer spends huge sums and develops novel furnace and tubing, and in the supreme end of the century, it is ripe that this respect technology has become.Novel furnace all adopts high temperature, short residence time(SRT) and low hydrocarbon partial pressure design, and selectivity and yield significantly improve, but high temperature also brings high coking rate.On tubing, high temperature alloy steel pipe such as Cr
25Ni
35And Cr
35Ni
45Deng containing the high alloy pipe of Cr, generally be used for cracking furnace pipe both at home and abroad, this type high temp non-corrosive metal pipe can form the passivation layer of high temperature resistant, low coking, Cr-Cr at short notice under the superheated vapor condition
2O
3Resist.
US 5630887,6436202,6824883,7056399 and 7156979; Among the CA2164021 high Cr, Ni alloy furnace tubes by adopting inwall are made high temperature, little oxygen atmosphere as handling with hydrogen or cracking tail gas saturation vapour; Make the Cr content of boiler tube internal surface be increased to 70～89% by former 30～45%; And the Ni that is prone to the catalysis green coke is about 1% by reducing to greater than 40%, and Fe reduces to about 1% by 8～20%, the effectively burnt generation of passive surface catalysis.In the ethane furnaceman of factory already uses, make the cycle of burning increase to 100～400 days by former about 40 days.Though above boiler tube process for treating surface is easy, the running time is long, and greater than 50～140 hours, and it was effective only ethane cracking furnace to be suppressed the high-temperature catalytic green coke.For other cracking than heavy hydrocarbon feeds, burnt at the resin that generates by on-catalytic below 650 ℃, only depend on the boiler tube surface-treated not reach and press down burnt purpose.
Adopt the online agent mode that adds of industry in ethane, petroleum naphtha and solar oil splitting gas, to add compounds such as burning agent K, Li, Ca, Mg and press down burnt passivator among US5358626, the US 6228253, can generate B at the high temperature tube wall
2O
3Or SiO
2Deng the compound of filming, the cycle of burning increased to 90～180 days by 40 days.Burn seriously all in nearly exit, quench tube rear portion at the empyreumatic position of restriction blowing out, and the radiation section noncoking.When US 6228253 proposed refinery gas pyrolysis, online steam added and burns agent, coke inhibitor schedule of operation, only needs about 6 hours can accomplish online burning, and the about 2 day time of burning program than conventional automatic or manual steam-air obviously shortens.
The passivation of having introduced organo phosphorous compounds among the US5354450,5360531,5779881 and 5954943 presses down Jiao and hydrolysis thereof or degradation production maybe be to the erosion of equipment with to the spinoffs such as poisoning of downstream catalyst.Think P contained compounds such as phosphoric acid trigalloyl piperidines and thiophosphatephosphorothioate to metal attack property little (it is little that the stainless steel batten is corroded thermal weight loss), but do not do to press down burnt experiment relatively.
To ethane experiment cracking tube, after tetrabutyl tin and SWS-F 221 pre-treatment, be that the coking rate of raw material is little about 3 times to the coking rate of no sulphur ethane cracking than the ethane that 200ppmDMS is arranged among the US 6497809, sulphur has abtragung to tin-silicon passivation layer.In the ethane experiment cracking tube of EP 0698654, single with tetrabutyl tin pre-treatment boiler tube, can make the coking amount of peeling off than about 5～10 times with the coking amount of peeling off of Sn/Si mixture process.Comprehensive Sn-Si presses down Jiao-decoking effect, and is single effective with the tin agent.But, cause the burnt dirt of follow-up Quench pipe to pile up unavoidably because the coking spall is a decorating film.
Test boiler tube with DMDS and SWS-F 221 mixture process among CN 1399760 and the WO 0121731; As Si/S=2: in the time of 1; Coking amount can be reduced to 66% of comparative quantity, through six circulations, and each pre-treatment 2 hours; Cracking 1 hour and air burn, and press down burnt rate and reduce to 36% by primary about 59%.
Existing press down burnt coke cleaning technology and stress onlinely to add table passivation in the agent pipe, or with the online steam coke cleaning of inorganic metal water liquid.The former is difficulty realization uniform coating; Often undesirable owing to adding the agent mode, cause the inorganic salt or the organic macromolecule thing that add in the agent to form salting stain or arborescens spot dirt at tube wall, quicken local Jiao's dirt and generate; Local superheating when subsequently online air is burnt reduces the boiler tube life-span.Same online steam burns difficult the realization the lower temperature district behind the cracking tube, the coke cleaning of chilling boiler tube.Though the steam coke cleaning has the thermo-negative reaction advantage, reach whole coke cleaning purposes, burn temperature than air and exceed about 200 ℃.Therefore keep 500～600 ℃ of quench zones to be difficult for reaching whole coke cleaning scale removal purposes.
Summary of the invention
The invention provides a kind of coke inhibitor for ethylene cracking, can effectively alleviate the coking of ethylene cracking tube, it is effective to press down Jiao, can obviously improve the ethylene cracking tube cycle of operation.Applied widely, use applicable to the Jiaozhuo that presses down of gaseous state lighter hydrocarbons, petroleum naphtha.
Described coke inhibitor for ethylene cracking, by the sulfocompound of 20-60%, the passivator of 5-10%, the membrane-forming agent of 1-10%, the stopper of 5-15%, the decoking agent of 1-10% and the solvent composition of 25-45%, above-mentioned consumption is weight percentage.
Described sulfocompound is dialkyl group two sulphur, dialkyl group sulphur, dialkyl phenol sulphur, diphenyl sulfide, diphenyl disulfide, thiophene or diformazan thiophene.
The alkyl of described dialkyl group two sulphur, dialkyl group sulphur, dialkyl phenol sulphur is methyl, ethyl, propyl group or butyl.Preferred sulfocompound is a DMDS.
Described passivator is triphenyl phosphite, triethyl-phosphite, dioctyl phenyl phosphate ester, tributyl phosphate, trilauryl trithiophosphite, diethyl phosphorothioate or phosphoric acid trigalloyl piperidines, preferred triphenyl phosphite, dioctyl phenyl phosphate ester.
Described membrane-forming agent is YSR 3286, gather di-ethyl siloxane, PSI, hexamethyl siloxanes or Hexaethyl siloxanes, preferred YSR 3286.
Described stopper is Resorcinol, p-ten.-butylcatechol, para benzoquinone, DBH 2,5 di tert butylhydroquinone, diethyl hydroxylamine, 2,2; 6,6-tetramethyl piperidine nitrogen oxygen free radical or 4-hydroxyl-2,2; 6,6-four phenylpiperidines-1-oxyradical, preferred Resorcinol, 2; 2,6, the 6-tetramethyl piperidine nitrogen oxygen free radical.
Described decoking agent is alkyl sodium salicylate, magnesium alkylsalicylate, thio-2 acid dimethyl ester, tin tetramethide, tetrabutyl tin or Mannich benzylamine.
Described solvent is kerosene, diesel oil, C
8-C
10Heavy aromatics, naphthane or methylnaphthalene.
Earlier solvent is joined in the reaction kettle, add sulfocompound, passivator, membrane-forming agent, stopper, decoking agent successively, at normal temperatures, stir insulation 1-3 hour, cold filtration promptly gets coke inhibitor for ethylene cracking.Generally the 10-1000ppm by the raw material weight ratio joins in the raw material, and coke inhibitor for ethylene cracking of the present invention can effectively be alleviated the coking of ethylene cracking tube, and it is effective to press down Jiao, can obviously improve the cracking cycle of operation and shorten air and burn the time spent.Applied widely, be applicable to that the Jiaozhuo that presses down of gaseous state lighter hydrocarbons, petroleum naphtha is used.
Description of drawings
Fig. 1 is for cracking and burn the experiment flow synoptic diagram, wherein
1 coke inhibitor for ethylene cracking recorder jar; 2 de-mineralized water recorder jars; 3 liquid starting material recorder jars; 4 gas raw material recorder jars, 5 air steel cylinders; 6,7,8 volume pumps; 13 under meters; 14 preheating temperature control sections; 16 cracking temperature control sections; The cold control section of 17 air; 18 water-cooled temperature control sections; Cracking tube is Φ 8 * 1 * 500mm stainless steel tube in the 16 cracking temperature control sections, and all joints are two logical, threeway, four-way stainless joint among the figure.
Embodiment
Further specify content of the present invention below in conjunction with embodiment.
Embodiment 1 coke inhibitor for ethylene cracking by DMDS 25%, triphenyl phosphite 10%, (TBN＞250mgKOH/g) magnesium alkylsalicylate 3% is formed with C10 heavy aromatic solvent 37% to gather di-ethyl siloxane 10%, p-ten.-butylcatechol 15%, high base number.
Embodiment 4 coke inhibitor for ethylene cracking are by dibutyl phenol sulphur 30%, trilauryl trithiophosphite 5%, hexamethyl siloxanes 9%, 2,2,6, and 6-tetramethyl piperidine nitrogen oxygen free radical 10%, tin tetramethide 3% and kerosene 43% are formed.
Embodiment 6 coke inhibitor for ethylene cracking by diphenyl sulfide 35%, triethyl-phosphite 7%, gather di-ethyl siloxane 8%, DBH 2,5 di tert butylhydroquinone 8%, tetrabutyl tin 4% and C9 heavy aromatic solvent 38% and form.
Embodiment 7 coke inhibitor for ethylene cracking are by diformazan thiophene 45%, tributyl phosphate 5%, PSI 4%, 4-hydroxyl-2,2,6, and 6-tetramethyl piperidine-1-oxyradical 6%, alkyl sodium salicylate (T109) 2% and C8 heavy aromatic solvent 38% are formed.
Evaluation method
When cracking stock is liquid phase; De-mineralized water in coke inhibitor in the coke inhibitor for ethylene cracking recorder jar 1, the de-mineralized water recorder jar 2 and the liquid phase feed in the liquid starting material recorder jar 3 are mixed through volume pump 6,7,8 metering backs respectively; Get into 14 vaporizations of preheating temperature control section; Get into the high-temperature zone-cracking furnace pipe of cracking temperature control section 16 then, hydrocarbon raw material generation scission reaction in pipe generates ethene and other product; For reducing the product loss that side reaction causes, splitting gas cooling rapidly in cold control section 17 of air and water-cooled temperature control section 18.
When cracking stock is gas phase; Coke inhibitor in phase feed in the gas raw material recorder jar 4 and the coke inhibitor for ethylene cracking recorder jar 1, the de-mineralized water in the de-mineralized water recorder jar 2 are respectively through mixing after under meter 13, volume pump 6,7 meterings; Get into 14 vaporizations of preheating temperature control section; Get into the high-temperature zone-cracking furnace pipe of cracking temperature control section 16 then, hydrocarbon raw material generation scission reaction in pipe generates ethene and other product; For reducing the product loss that side reaction causes, splitting gas cooling rapidly in cold control section 17 of air and water-cooled temperature control section 18.
Experimental procedure
(1) purges: switch different pipelines, drive the air in the device out of system.
(2) preheating: open temperature controlling system, and instrument is set to service temperature, de-mineralized water is adjusted to suitable flow, treat that its temperature out is stable.
(3) charging: open the volume pump of raw material and coke inhibitor, charging after stablizing, is collected cracked gas and tail oil.
(4) change raw material and add the coke inhibitors of different amounts, repeat above step (1)-(3), obtain blank (promptly not mixing coke inhibitor) coke yield respectively, add the productive rate of coke behind the coke inhibitor.
Press down burnt rate y%=(coke yield after blank coke yield-Jia agent)/blank coke yield relatively
Appreciation condition
Raw material: the ethane residence time: 0.28s thinning ratio: 0.3
The petroleum naphtha residence time: 0.26s thinning ratio: 0.6
Adopt above-mentioned evaluation method that embodiment 1-7 gained coke inhibitor for ethylene cracking is estimated, and with market on the general coke inhibitor for ethylene cracking A that is used for compare, test-results is seen table 1.
Table 1 alkene cracking coke inhibitor test-results
Claims (2)
1. coke inhibitor for ethylene cracking, it is characterized in that: by the sulfocompound of 20-60%, the passivator of 5-10%, the membrane-forming agent of 1-10%, the stopper of 5-15%, the decoking agent of 1-10% and the solvent composition of 25-45%, above-mentioned consumption is weight percentage;
Described sulfocompound is dialkyl group two sulphur, dialkyl group sulphur, dialkyl phenol sulphur, diphenyl sulfide, diphenyl disulfide, thiophene or diformazan thiophene;
Described passivator is triphenyl phosphite, triethyl-phosphite, dioctyl phenyl phosphate ester, tributyl phosphate, trilauryl trithiophosphite, diethyl phosphorothioate or phosphoric acid trigalloyl piperidines;
Described membrane-forming agent is YSR 3286, gather di-ethyl siloxane, PSI, hexamethyl siloxanes or Hexaethyl siloxanes;
Described stopper is Resorcinol, p-ten.-butylcatechol, para benzoquinone, DBH 2,5 di tert butylhydroquinone, diethyl hydroxylamine, 2,2,6,6-tetramethyl piperidine nitrogen oxygen free radical or 4-hydroxyl-2,2,6,6-tetramethyl piperidine-1-oxyradical;
Described decoking agent is alkyl sodium salicylate, magnesium alkylsalicylate, thio-2 acid dimethyl ester, tin tetramethide, tetrabutyl tin or Mannich benzylamine;
Described solvent is kerosene, diesel oil, C
8-C
10Heavy aromatics, naphthane or methylnaphthalene.
2. coke inhibitor for ethylene cracking according to claim 1 is characterized in that: the alkyl in described dialkyl group two sulphur, dialkyl group sulphur, the dialkyl phenol sulphur is methyl, ethyl, propyl group or butyl.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102641926A CN101747927B (en) | 2009-12-31 | 2009-12-31 | Coke inhibitor for ethylene cracking |
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|---|---|---|---|
| CN2009102641926A CN101747927B (en) | 2009-12-31 | 2009-12-31 | Coke inhibitor for ethylene cracking |
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| CN101747927A CN101747927A (en) | 2010-06-23 |
| CN101747927B true CN101747927B (en) | 2012-08-08 |
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|---|---|---|---|---|
| CN101880544A (en) * | 2010-07-01 | 2010-11-10 | 华东理工大学 | Composite method for inhibiting ethylene cracking device from coking |
| CN102277220A (en) * | 2011-07-08 | 2011-12-14 | 唐东波 | On-line scavenger for coking of straw briquettes |
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| CN103421531B (en) * | 2013-07-19 | 2015-08-12 | 金昌市万隆实业有限责任公司 | One alleviates cracking furnace pipe method for coke |
| US10047020B2 (en) | 2013-11-27 | 2018-08-14 | Siluria Technologies, Inc. | Reactors and systems for oxidative coupling of methane |
| CN110655437B (en) | 2014-01-08 | 2022-09-09 | 鲁玛斯技术有限责任公司 | System and method for ethylene to liquids |
| US10377682B2 (en) | 2014-01-09 | 2019-08-13 | Siluria Technologies, Inc. | Reactors and systems for oxidative coupling of methane |
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| US10793490B2 (en) | 2015-03-17 | 2020-10-06 | Lummus Technology Llc | Oxidative coupling of methane methods and systems |
| US9334204B1 (en) | 2015-03-17 | 2016-05-10 | Siluria Technologies, Inc. | Efficient oxidative coupling of methane processes and systems |
| US20160289143A1 (en) | 2015-04-01 | 2016-10-06 | Siluria Technologies, Inc. | Advanced oxidative coupling of methane |
| US9328297B1 (en) | 2015-06-16 | 2016-05-03 | Siluria Technologies, Inc. | Ethylene-to-liquids systems and methods |
| EP3786138A1 (en) | 2015-10-16 | 2021-03-03 | Lummus Technology LLC | Oxidative coupling of methane |
| CA3019396A1 (en) | 2016-04-13 | 2017-10-19 | Siluria Technologies, Inc. | Oxidative coupling of methane for olefin production |
| EP3554672A4 (en) | 2016-12-19 | 2020-08-12 | Siluria Technologies, Inc. | Methods and systems for performing chemical separations |
| EP3630707B1 (en) | 2017-05-23 | 2023-09-06 | Lummus Technology LLC | Integration of oxidative coupling of methane processes |
| US10836689B2 (en) | 2017-07-07 | 2020-11-17 | Lummus Technology Llc | Systems and methods for the oxidative coupling of methane |
| CN117603726A (en) * | 2024-01-17 | 2024-02-27 | 江阴盛源科技有限公司 | Coking inhibitor for ethylene unit cracking furnace and preparation method thereof |
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