CN102311757B - Method for improving yield of delayed coking liquid product - Google Patents
Method for improving yield of delayed coking liquid product Download PDFInfo
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- CN102311757B CN102311757B CN 201010211572 CN201010211572A CN102311757B CN 102311757 B CN102311757 B CN 102311757B CN 201010211572 CN201010211572 CN 201010211572 CN 201010211572 A CN201010211572 A CN 201010211572A CN 102311757 B CN102311757 B CN 102311757B
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- oil
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- inorganic materials
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/04—Other carbonising or coking processes; Features of destructive distillation processes in general using charges of special composition
- C10B57/06—Other carbonising or coking processes; Features of destructive distillation processes in general using charges of special composition containing additives
Abstract
The invention relates to a method for improving a yield of a delayed coking liquid product. A liquid-increasing addition agent is added into a charged material of a coking tower; by taking the mass of raw oil as a standard, the adding amount of the liquid-increasing addition agent is 0.01-2%; the liquid-increasing addition agent contains 5-15 m% of acidified inorganic material, 5-15 m% of oil-soluble free radical initiator and 70-90 m% of dispersant; the acidified inorganic material is obtained by treating the inorganic material the Al2O3 mass content of which is not less than 15% by utilizing an inorganic strong acid solution, then drying, baking and crushing; the average grain diameter of the acidified inorganic material is not more than 300 microns; and the viscosity of the dispersant at 100 DEG C is not less than 30 mm<2>/s. According to the method provided by the invention, the yield of the delayed coking liquid product is improved, the yield of the coke is reduced, and the distribution of the liquid product is improved.
Description
Technical field
The present invention relates to a kind of method that improves production efficiency of delayed coking liquid product.
Background technology
Along with a large amount of consumption of light crude, the heaviness trend of world petroleum resource is constantly aggravated, and the demand of light-end products increases day by day, so the upgrading of heavy oil and deep processing become one of important topic that Petrochemical Enterprises faces.At present, the deep processing method of heavy oil is still take hot-work as main, and delayed coking is wherein most important a kind of.The liquid yield of delay coking process can be lower during the processing poor residuum in 70% left and right, and coke yield can reach 30%, is the major objective of this technique so improve the coking liquid product yield.
In order to improve the yield of light oil of delayed coking, reduce coke yield, the investigator has proposed many methods both at home and abroad, mainly contains two classes: the one, the coking process flow process is improved; The 2nd, add auxiliary agent in stock oil, as thinner, increase liquor.Adding and increasing liquor is a kind of effective way that improves production efficiency of delayed coking liquid product, increases the Main Function of liquor: the one, and promote free radical to generate, increase the cracking level of raw material; The 2nd, stop the free radical condensation, reduce the probability of macromolecular radical condensation coking.Proposing to add massfraction in the delayed coking charging as Texaco company is the traditional radical initiator of chain reaction delivery agent (as mercaptan, tetracol phenixin etc.) and 0.1% left and right of 0.5% left and right, the Mobil oil company proposes to add free radical terminator in the delayed coking charging, and purpose is all to reduce the further condensation of unstable hydrocarbon type free base that thermally splitting produces.
Summary of the invention
A kind of method that improves production efficiency of delayed coking liquid product is added with in the charging of coke drum and increases the liquid auxiliary agent, and take the quality of stock oil as benchmark, the add-on that increases the liquid auxiliary agent is 0.01%～2%; Describedly increase acidifying inorganic materials, the oil soluble radical initiator of 5m%～15m% and the dispersion agent of 70m%～90m% that the liquid auxiliary agent contains 5m%～15m%; Described acidifying inorganic materials is to process Al with the inorganic acid aqueous solution
2O
3The inorganic materials of content 〉=15m%, and drying, roasting, pulverizing and obtain the median size of acidifying inorganic materials≤300 μ m; Described dispersion agent is at the viscosity 〉=30mm of 100 ℃
2/ s.
Take the quality of stock oil as benchmark, the add-on that increases the liquid auxiliary agent is 0.02%～1%.
The median size of described acidifying inorganic materials is preferred≤100 μ m.Median size in the present invention is the linear averaging particle diameter, adopts the sedimentation particle size analyzer determination.
In described inorganic materials, Al
2O
3Content is preferred 〉=30m%, and more preferably 〉=40m%.Described inorganic materials can be one or more in aluminium hydroxide, aluminum oxide, clay, zeolite and aluminate, is preferably one or more in pseudo-boehmite, gama-alumina, calcium aluminate, y-type zeolite, kaolin and polynite.
Described inorganic acid can be hydroiodic acid HI, perchloric acid, Hydrogen bromide, hydrochloric acid, nitric acid or sulfuric acid, is preferably hydrochloric acid, nitric acid or sulfuric acid.
Described oil soluble radical initiator is preferably one or more in alkyl peroxide, alkyl peroxide and peroxyester.
The viscosity upper limit of dispersion agent is relevant with the stock oil of heavy oil thermal conversion process, as basic general knowledge, can better be scattered in stock oil in order to make auxiliary agent, and the viscosity of dispersion agent should be less than the raw material oil viscosity.In described dispersion agent, the total content of naphthenic hydrocarbon and light aromatic hydrocarbons is preferred 〉=50m%, and wherein light aromatic hydrocarbons refers to monocycle, dicyclo and thrcylic aromatic hydrocarbon.Described dispersion agent is preferably naphthane, 9,10-dihydroanthracene, 9, and the 10-dihydro is luxuriant and rich with fragrance, methylnaphthalene, lube oil finishing oil, catalytically cracked oil etc.In preferred embodiments of the present invention, use the dispersion agent that is rich in naphthenic hydrocarbon and light aromatic hydrocarbons, can stop on the one hand the polymerization of aromatic hydrocarbons macromole to generate coke precursor, thereby reduce the productive rate of coke, can promote heat cracking reaction on the other hand.
The described preparation method who increases the liquid auxiliary agent comprises:
(1) process inorganic materials in the inorganic acid aqueous solution, separate drying, roasting;
(2) sample that step (1) is obtained is crushed to median size≤300 μ m;
(3) sample dispersion that step (2) is obtained is in the dispersion agent that contains the oil soluble radical initiator.
In preferred situation, front in step (1), with described inorganic materials roasting 4h at least between 400～650 ℃.
In step (1), described inorganic acid is hydroiodic acid HI, perchloric acid, Hydrogen bromide, hydrochloric acid, nitric acid or sulfuric acid, and the concentration of the inorganic acid aqueous solution is 1～5mol/L, is preferably 1～3mol/L; Preferred 0.5～4h of acid treatment time, treatment temp is preferably 60～90 ℃; Drying temperature is preferably 100～120 ℃, is preferably 4～12h time of drying; Preferred 400～650 ℃ of maturing temperature, the preferred 4～8h of roasting time.
In step (2), the sample that preferably step (1) is obtained is crushed to median size≤100 μ m.
In step (3), preferably adopt the mode of high-speed stirring, the sample dispersion that step (2) is obtained is in the dispersion agent that contains the oil soluble radical initiator.The method of disperseing with high-speed stirring belongs to prior art.
In the present invention, both the described liquid auxiliary agent that increases can be joined in stock oil in advance, then with stock oil input delay coker; Also can or add at the bottom of coke drum before the Fractionator Bottom of delayed coking unit, process furnace pump, preferably add to increase the liquid auxiliary agent at the bottom of the coke drum of delayed coking unit.
Temperature of reaction of the present invention is 470～520 ℃, preferred 490～515 ℃ (furnace outlet temperature).
Described stock oil includes but not limited to long residuum, vacuum residuum, catalytically cracked oil, viscosity breaking oil and viscous crude, and viscous crude wherein comprises common heavy oil, special viscous crude and super viscous crude.Described viscous crude is the criteria classification by China, and take viscosity as the first index, density is auxiliary characteristics.
The present invention can significantly improve production efficiency of delayed coking liquid product, simultaneously the decrease coke yield by add a kind of new liquid auxiliary agent that increases in the delayed coking reaction logistics.To increase the liquid auxiliary agent and add at the bottom of the coke drum fashionablely, not only improve production efficiency of delayed coking liquid product, also improve the liquid product distribution.
Embodiment
Further set forth by the following examples the present invention.
Test raw materials used oil nature and see Table 1.The thermal conversion reaction that increases liquid auxiliary agent A～D the results are shown in Table 2 and table 3.Different positions at delayed coking unit adds the commercial test results after increasing the liquid auxiliary agent to list in table 4.
Embodiment 1
Get the baked kaolin of 50g, use the HCl of 1mol/L to process 2h at 70 ℃, then at 120 ℃ of dry 4h, 550 ℃ of roasting 4h obtain the acid-treated kaolin of salt, are crushed into 120 orders (120 μ m) standby, are designated as A-1.
By A-1: dicumyl peroxide (DCP): the mass ratio of naphthane=5: 5: 90 mixes the three, stirs 30min at 800rpm and obtains auxiliary agent A.
The benchmark test of auxiliary agent carries out on the static heat conversion system in laboratory, add a certain amount of stock oil first (character sees Table 1) and auxiliary agent A (take the quality of stock oil as benchmark in reactor, add-on is 200 μ g/g), then rise to 470 ℃ of temperature of reaction, stop 30min.Crackate liquid product after cooling enters holding tank, and gaseous product is through the gas meter metered volume, and sedimentation of coke is at reactor bottom, and test-results sees Table 2.
As can be seen from Table 2,470 ℃, add the auxiliary agent A of 200 μ g/g, liquid product yield is 64.67%, improves 0.8 percentage point than Comparative Examples 1; Coke yield is 26.28%, compares ratio 1 and descends 1 percentage point.
Comparative Examples 1
Comparative Examples 1 is not added any auxiliary agent, adopts reaction conditions and the raw material identical with embodiment 1, and test-results sees Table 2.
As can be seen from Table 2, do not add any auxiliary agent, at 470 ℃, the coke yield of stock oil is 27.28%, and liquid product yield is 63.87%.
Embodiment 2
Get γ-Al of 50g
2O
3, with the H of 2mol/L
2SO
4Process 2h at 80 ℃, at 120 ℃ of dry 4h, 550 ℃ of roasting 4h obtain the gama-alumina of vitriolization, are crushed into 120 orders (120 μ m) standby, are designated as B-1.
B-1 in mass ratio: radical initiator dibenzoyl peroxide (BPO): the mass ratio of 9,10-dihydroanthracene=5: 10: 85 mixes the three, first stirs 30min at 800rpm, obtains auxiliary agent B.
Add auxiliary agent B in the stock oil first, take the quality of stock oil as benchmark, add-on is 500 μ g/g, and reaction conditions is with embodiment 1, and test-results is listed in table 2.As can be seen from Table 2, compare with Comparative Examples 1, liquid product yield improves 0.9 percentage point, reaches 64.77%; Coke yield descends 1.2 percentage points, reaches 26.08%.
Embodiment 3
Get the illiteracy holder soil of 50g, with the H of 2mol/L
2SO
4Process 2h at 80 ℃, at 120 ℃ of dry 4h, 550 ℃ of roasting 4h, obtain the illiteracy holder soil of vitriolization, be crushed into 150 orders (100 μ m) standby, be designated as C-1;
Press C-1: ditertiary butyl peroxide (DTBP): 9,10-dihydro is luxuriant and rich with fragrance=and the mass ratio of 10: 5: 85 mixes the three, stirs 20min at 1000rpm, obtains auxiliary agent C.
Add auxiliary agent C in the stock oil first, take the quality of stock oil as benchmark, add-on is 1000 μ g/g, and reaction conditions is with embodiment 1, and test-results sees Table 2.
As can be seen from Table 2, compare with Comparative Examples 1, add the auxiliary agent C of 1000 μ g/g, the productive rate of coke is 25.28%, has descended 2 percentage points, and liquid product yield increases by 1.6 percentage points, increases to 64.47%.
Embodiment 4
Get the Y molecular sieve of 50g, with the HNO of 3mol/L
3Process 2h at 70 ℃, at 120 ℃ of dry 4h, 550 ℃ of roasting 4h obtain the Y molecular sieve of nitric acid treatment, are crushed into 200 orders (70 μ m) standby, are designated as D-1.
By D-1: ditertiary butyl peroxide (DTBP): the mass ratio of lube oil finishing oil=15: 5: 80 mixes the three, stirs 30min at 800rpm, obtains auxiliary agent D.In lube oil finishing oil, the mass content sum of naphthenic hydrocarbon and light aromatic hydrocarbons is 63%.
Add auxiliary agent D in the stock oil first, take the quality of stock oil as benchmark, add-on is 3000 μ g/g, and reaction conditions is with embodiment 1, and test-results sees Table 2.
As can be seen from Table 2, adding the productive rate of 3000 μ g/g auxiliary agent D coke is 22.78, has descended 4.5 percentage points than Comparative Examples 1, and liquid product yield is 67.87%, increases by 4 percentage points than Comparative Examples 1.
Embodiment 5
Get the baked kaolin of 50g, with the HNO of 2mo l/L
3Process 2h at 70 ℃, at 120 ℃ of dry 4h, 550 ℃ of roasting 4h obtain the kaolin of nitric acid treatment, are crushed into 150 orders (100 μ m) standby, are designated as E-1.
By E-1: ditertiary butyl peroxide (DTBP): the mass ratio of catalytic slurry=5: 15: 80 mixes the three, first stirs 30min at 800rpm, obtains auxiliary agent E.The mass content sum of the naphthenic hydrocarbon in catalytic slurry and light aromatic hydrocarbons is 70%.
Add auxiliary agent E in the stock oil first, take the quality of stock oil as benchmark, add-on is 3000 μ g/g, and reaction conditions is with embodiment 1, and test-results sees Table 2.
As can be seen from Table 2, add 3000 μ g/g auxiliary agent E, the productive rate of coke descends 1.5 percentage points, and liquid product yield increases by 1.15 percentage points.
Embodiment 6
Test method is identical with embodiment 1, just uses raw material second (character sees Table 1), and 490 ℃ of temperature of reaction take the quality of stock oil as benchmark, add the auxiliary agent D of 5000 μ g/g, and test-results sees Table 3.
As can be seen from Table 3, after adding 5000 μ g/g auxiliary agent D, coke yield descends 3.9 percentage points, and liquid product yield improves 3.28 percentage points.
Comparative Examples 2
Comparative Examples 2 is not added any auxiliary agent, adopts reaction conditions and the raw material identical with embodiment 6, and test-results sees Table 3.
As can be seen from Table 3, do not add auxiliary agent, at 490 ℃, the coke yield of raw material second is 28.58%, and liquid product yield is 62.67%.
Embodiment 7～9 and Comparative Examples 3
The processing condition of coking industry test are: 500 ℃ of heating raw materials heater outlet temperatures, working pressure are 0.17Mpa, recycle ratio 0 (w/w).Coke drum coke long-pending full rear (approximately 18h) stops charging, and adustion 4 hours is removed fugitive constituent.Embodiment 7～9 for respectively before Fractionator Bottom, process furnace pump or coke drum bottom add and increase the liquid auxiliary agent, the add-on of auxiliary agent is 300 μ g/g (take the quality of stock oil as benchmark); Comparative Examples 3 does not add any auxiliary agent.Reaction result is listed in table 4.
As shown in Table 4, before separation column bottom, process furnace pump or add the auxiliary agent D of 300 μ g/g that the delay coking process liquid product yield is improved at the bottom of coke drum, compare with Comparative Examples 3, improve respectively 1.13,1.57 and 1.85 percentage points; Lightweight oil (gasoline+diesel oil) yield improves respectively 0.35,1.01,2.05 percentage point.Compare with Comparative Examples 3, coking yield reduces respectively 1.40,1.95 and 2.02 percentage points.
Table 1
Table 2
Table 3
Table 4
Total liquid product yield comprises gasoline, diesel oil and wax oil yield sum, and yield of gasoline comprises C
5, C
6With the cut yield sum of initial boiling point less than 180 ℃.
Claims (12)
1. a method that improves production efficiency of delayed coking liquid product, is characterized in that, is added with in the charging of coke drum to increase the liquid auxiliary agent, and take the quality of stock oil as benchmark, the add-on that increases the liquid auxiliary agent is 0.01%～2%; Describedly increase acidifying inorganic materials, the oil soluble radical initiator of 5m%～15m% and the dispersion agent of 70m%～90m% that the liquid auxiliary agent contains 5m%～15m%; Described acidifying inorganic materials is to process Al with the inorganic acid aqueous solution
2O
3The inorganic materials of content 〉=15m%, and drying, roasting, pulverizing and obtain the median size of acidifying inorganic materials≤300 μ m; Described dispersion agent is at the viscosity 〉=30mm of 100 ℃
2/ s.
2. in accordance with the method for claim 1, it is characterized in that, take the quality of stock oil as benchmark, the add-on that increases the liquid auxiliary agent is 0.02%～1%.
3. in accordance with the method for claim 1, it is characterized in that, the median size of described acidifying inorganic materials is preferred≤100 μ m.
4. in accordance with the method for claim 1, it is characterized in that, described inorganic materials is one or more in aluminium hydroxide, aluminum oxide, clay, zeolite and aluminate.
5. in accordance with the method for claim 4, it is characterized in that, described inorganic materials is one or more in pseudo-boehmite, gama-alumina, calcium aluminate, y-type zeolite, kaolin and polynite.
6. in accordance with the method for claim 1, it is characterized in that, described inorganic acid is hydroiodic acid HI, perchloric acid, Hydrogen bromide, hydrochloric acid, nitric acid or sulfuric acid.
7. in accordance with the method for claim 1, it is characterized in that, described oil soluble radical initiator is one or more in alkyl peroxide and peroxyester.
8. in accordance with the method for claim 1, it is characterized in that, in described dispersion agent, the total content of naphthenic hydrocarbon and light aromatic hydrocarbons is preferred 〉=50m%.
9. in accordance with the method for claim 1, it is characterized in that, described dispersion agent is naphthane, 9,10-dihydroanthracene, 9, and the 10-dihydro is luxuriant and rich with fragrance, methylnaphthalene, lube oil finishing oil or catalytically cracked oil.
10. in accordance with the method for claim 1, it is characterized in that, the described liquid auxiliary agent that increases is joined in stock oil in advance, then with stock oil input delay coker; Perhaps before the Fractionator Bottom of delayed coking unit, process furnace pump or add at the bottom of coke drum and increase the liquid auxiliary agent.
11. in accordance with the method for claim 1, it is characterized in that, temperature of reaction is 470～520 ℃.
12. in accordance with the method for claim 1, it is characterized in that, described stock oil is long residuum, vacuum residuum, catalytically cracked oil, viscosity breaking oil or viscous crude.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4298455A (en) * | 1979-12-31 | 1981-11-03 | Texaco Inc. | Viscosity reduction process |
| US4394250A (en) * | 1982-01-21 | 1983-07-19 | Chevron Research Company | Delayed coking process |
| CN1487056A (en) * | 2002-10-01 | 2004-04-07 | 曹炳铖 | Method of raising liquid yield during delayed coking |
| CN1560198A (en) * | 2004-03-04 | 2005-01-05 | 沈阳工业大学 | Additive for enhancing and delaying light oil recovery rate of coke apparatus |
| CN1928021A (en) * | 2006-09-06 | 2007-03-14 | 中国石油化工集团公司 | Auxiliary agent capable of improving delayed coking liquid yield, preparation method and application thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US31726A (en) * | 1861-03-19 | Whole | ||
| US7067053B2 (en) * | 2002-08-16 | 2006-06-27 | Intevep, S.A. | Additives for improving thermal conversion of heavy crude oil |
-
2010
- 2010-06-29 CN CN 201010211572 patent/CN102311757B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4298455A (en) * | 1979-12-31 | 1981-11-03 | Texaco Inc. | Viscosity reduction process |
| US4394250A (en) * | 1982-01-21 | 1983-07-19 | Chevron Research Company | Delayed coking process |
| CN1487056A (en) * | 2002-10-01 | 2004-04-07 | 曹炳铖 | Method of raising liquid yield during delayed coking |
| CN1560198A (en) * | 2004-03-04 | 2005-01-05 | 沈阳工业大学 | Additive for enhancing and delaying light oil recovery rate of coke apparatus |
| CN1928021A (en) * | 2006-09-06 | 2007-03-14 | 中国石油化工集团公司 | Auxiliary agent capable of improving delayed coking liquid yield, preparation method and application thereof |
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