CN104560195B - A kind of Virahol urea dewaxing method - Google Patents
A kind of Virahol urea dewaxing method Download PDFInfo
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- CN104560195B CN104560195B CN201310503571.2A CN201310503571A CN104560195B CN 104560195 B CN104560195 B CN 104560195B CN 201310503571 A CN201310503571 A CN 201310503571A CN 104560195 B CN104560195 B CN 104560195B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/02—Recovery of petroleum waxes from hydrocarbon oils; Dewaxing of hydrocarbon oils
- C10G73/06—Recovery of petroleum waxes from hydrocarbon oils; Dewaxing of hydrocarbon oils with the use of solvents
- C10G73/08—Organic compounds
- C10G73/22—Mixtures or organic compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
- C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
- C10G53/04—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one extraction step
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The present invention relates to a kind of Virahol urea aqueous solution by dewaxing method, specifically comprise following content, enter reactor after stock oil and Virahol aqueous solution of urea mix and carry out complex reaction, described reactor operates at reduced pressure conditions, the vapor phase stream effluent of reactor head returns reactor through cooling Posterior circle, the reaction product part Returning reactor that reactor bottom obtains, remainder goes complex compound sedimentation washing tower to carry out later separation process.The inventive method adopts decompression operation, utilize the Virahol in Virahol aqueous solution of urea, water vapor is when being gaseous state by liquid state, absorb the normal paraffin complex reaction liberated heat in urea and stock oil, thus meet the requirement of complex reaction to temperature, need not additionally introduce other heat-eliminating mediums, avoid in prior art and use a large amount of low temperature underground water to control temperature of reaction, save groundwater resource, this technology can also be applied in the relatively deficient area of water resources.
Description
Technical field
The present invention relates to a kind of process for dewaxing, particularly a kind of Virahol aqueous solution of urea complex reaction process for dewaxing.
Background technology
Urea dewaxing technology utilizes urea molecule to contact the spirrillum hexagonal crystallization will formed around normal paraffin with normal paraffin, formed and the ultimate principle of the immiscible complex compound of oil, thus by normal paraffin and separating of oil.The duct of spirrillum hexagonal crystallization is 0.525nm, also can regard the organic molecule sieve that aperture is single as.
Virahol urea dewaxing is that urea and a certain proportion of water, Virahol mix, and heated mixt to urea dissolves the uniform solution of formation completely, adding dewaxed feedstock makes itself and Virahol aqueous solution of urea fully mix, be conducive to contacting of urea and normal paraffin, then the temperature of reaction mixture is reduced gradually, urea and normal paraffin carry out reacting the complex compound being formed and be insoluble to oil, and its normal paraffin (wax) is deviate from from oil.Along with the decline of temperature of reaction, the amount of deviating from normal paraffin (dewaxing) increases, until reaction final temperature.
The range of reaction temperature of current Virahol urea dewaxing process is that between normal temperature ~ 70 DEG C, complex reaction carries out in double-tube reactor, uses water as heat-eliminating medium.Be reaction mixture in pipe, chuck water flowing, adverse current indirect heat exchange, because reaction final temperature is lower at 20 ~ 30 DEG C, the temperature of the water coolant of needs is lower.Full scale plant is in order to ensure stable water temperature water source, and adopt underground water as heat-eliminating medium, water temperature remains on 11 ~ 13 DEG C throughout the year, and the water yield of needs is large especially, if particularly between water temperature and reaction final temperature the temperature difference less, the water yield of needs is more.CN201110081607.3 water supply pump extracts low temperature 5 DEG C of water out from cold water tank, deliver to the heat exchange of complex reaction double-pipe crystallizer shell side, about temperature rise to 20 DEG C, then after full liquid type evaporation sled block and liquefied ammonia heat exchange cool, enter cold water tank again, form a closed cycle; Adopt liquefied ammonia process of refrigeration, add investment and the energy consumption of device.
Due to isopropanol water solution urea dewaxing technology, when using water as refrigeration agent, the cooling water inflow that reactive system needs is a lot, and water temperature requires also lower, and heat exchange mode is indirect heat exchange, the wall of reactor temperature directly contacted with heat-eliminating medium water can be caused lower than reactor temperature, and the normal paraffin in urea and stock oil can react on wall, forms complex compound, and be attached on tube wall, form knot wall phenomenon, reduce heat transfer effect, easily make line clogging for a long time and affect normal production.Industrial pipe in adopt spiral scraper, at any time removing tube wall on complex compound.And China is again a poor-water state, water resources is relatively poor, also constrains the development of this technology.
Summary of the invention
The present invention is directed to the deficiency that existing Virahol urea aqueous solution by dewaxing complex reaction exists, adopt Virahol to make heat-eliminating medium, heat absorption of vaporizing when utilizing isopropyl alcohol and water to form azeotrope, reaches the requirement of the many temperature of complex reaction, not only save a large amount of water at low temperature resource, and simplify technological process.
The invention provides a kind of Virahol urea aqueous solution by dewaxing method, enter reactor after stock oil and Virahol aqueous solution of urea mix and carry out complex reaction, described reactor operates at reduced pressure conditions, the vapor phase stream effluent of reactor head returns reactor through cooling Posterior circle, the reaction product part Returning reactor that reactor bottom obtains, remainder goes complex compound sedimentation washing tower to carry out later separation process.
According to Virahol urea aqueous solution by dewaxing method of the present invention, the initial boiling point of described stock oil is 170 DEG C ~ 200 DEG C, and final boiling point is 320 DEG C ~ 350 DEG C.In described Virahol aqueous solution of urea, urea concentration is 28wt% ~ 38wt%, and isopropyl alcohol concentration is 40wt% ~ 55wt%, and comparatively suitable urea concentration is 30wt% ~ 35wt%, and isopropyl alcohol concentration is 46wt% ~ 50wt%.Described stock oil and Virahol aqueous solution of urea feed weight, than being 1:5 ~ 1:30, are preferably 1:8 ~ 1:20.
According to Virahol urea aqueous solution by dewaxing method of the present invention, reactor feed temperature is 60 DEG C ~ 80 DEG C, and reaction final temperature is 20 DEG C ~ 32 DEG C, and preferred feedstock temperature is 65 DEG C ~ 70 DEG C, and reaction final temperature is 25 DEG C ~ 30 DEG C.
According to Virahol urea aqueous solution by dewaxing method of the present invention, reactor operating pressure 20 ~ 50kPa, preferably 30 ~ 40kpa.
According to Virahol urea aqueous solution by dewaxing method of the present invention, described incoming mixture enters along the tangential direction of reactor, plays stirring action to reaction mixture, is conducive to the carrying out of complex reaction.
According to Virahol urea aqueous solution by dewaxing method of the present invention, the vapor phase stream effluent of reactor head loops back reactor from the position of 2 ~ 6 different heights in the reactor lower part reactant bed of material along the tangential direction of reactor after cooling.
According to Virahol urea aqueous solution by dewaxing method of the present invention, described condenser can be tube in-tube condenser or shell and tube cooler.
In the inventive method, complex compound sedimentation washing tower later separation treating processes is as follows, remainder complex compound enters complex compound sedimentation washing tower, countercurrent washing is carried out with the washing oil entered from complex compound sedimentation washing tower bottom, tower top obtains dewaxing liquid, the complex compound through washing is obtained at the bottom of tower, complex compound after washing oil washing enters complex decomposes system through pipeline, and in complex decomposes system through thermal degradation be wax liquid and urine, urine is circulated to urine tank, and dewaxing liquid and wax liquid obtain pressed oil and liquid wax respectively through washing, fractionation.Washing dewaxing liquid and wax liquid obtain containing alcohol water, through binary azeotropic distillation, obtain the Virahol of 80 ~ 85wt%, then carry out ternary azeotropic distill >=96wt% Virahol is circulated to urine, tank.
Compared with prior art, in Virahol urea aqueous solution by dewaxing method of the present invention, have the following advantages by making heat-eliminating medium tool with Virahol:
(1) in the inventive method, because reactor adopts decompression operation, under feeding temperature condition, can vaporize after isopropyl alcohol and water in Virahol aqueous solution of urea enters reactor, when isopropyl alcohol and water is gaseous state by liquid state, the normal paraffin complex reaction liberated heat in urea and stock oil can be absorbed, thus meet the requirement of complex reaction to temperature.Need not additionally introduce other heat-eliminating mediums in the inventive method, only rely on the character of isopropyl alcohol and water in reaction raw materials, adopt suitable reaction conditions just to meet the requirement of complex reaction to temperature.Also avoid in prior art and use a large amount of low temperature underground water to control temperature of reaction; save a large amount of valuable groundwater resource; can not pollute underground water, better protection is provided to groundwater resource, this technology can also be applied in the relatively deficient area of water resources.
(2) in the inventive method, incoming mixture enters along the tangential direction of reactor, certain stirring action is served to reaction mixture, the normal paraffin in urea and stock oil can be made to distribute in aqueous isopropanol more evenly and then form crystallization, avoid and adopt water as knot wall phenomenon occurs during heat-eliminating medium on shell and tube-type reactor wall, reaction mixture lowering temperature uniform, what be conducive to that complex reaction carries out is more abundant.
(3) in the inventive method, reactor top mixture is derived from reactor head, enter through the tangential direction of condensing cooling from the position of 2 ~ 6 different heights in the reactor lower part reactant bed of material along reactor, make its reactor content layer formation temperature gradient from top to bottom, be conducive to the viscosity reducing reactant, have further stirring action to reaction mixture, make it more even, what be conducive to that complex reaction carries out is more abundant, is also conducive to the separation of complex compound.
Accompanying drawing explanation
Fig. 1: a kind of schema of Virahol urea dewaxing method of the present invention.
Embodiment
Further illustrate technical scheme of the present invention and effect below in conjunction with drawings and Examples, but these embodiments can't limit the scope of the invention.
As shown in Figure 1, reactor 3 is entered through pipeline along reactor tangential direction after Virahol aqueous solution of urea 1 in urine tank mixes with stock oil 2, reactor 3 top is connected with vaccum-pumping equipment 13, for ensureing that reactor is operate under reduced pressure, isopropyl alcohol and water in charging Virahol aqueous solution of urea can be vaporized with this understanding, vaporescence can absorb sensible heat and the complex reaction liberated heat of mixture, and then meets the requirement of complex reaction to temperature.Reactor head effluent 4 loops back reactor from the position of 4 different heights in the reactor lower part reactant bed of material along the tangential direction of reactor after condenser 5 cools.The reaction product 6 that reactor bottom obtains can be divided into two portions, wherein a part of 7 Returning reactor devices, remainder 8 enters complex compound sedimentation washing tower 10, countercurrent washing is carried out with the washing oil 9 entered from complex compound sedimentation washing tower bottom, tower top obtains dewaxing liquid 11, tower reactor obtains the complex compound 12 through washing, through washing oil washing after complex compound 12 through pipeline enter complex decomposes system 14 and in complex decomposes system through thermal degradation be urine 15 and wax liquid 16, urine 15 is circulated to urine tank 1, dewaxing liquid 11 and wax liquid 16 are through washing, fractionation obtains pressed oil and liquid wax respectively.
Embodiment 1
In the present embodiment, raw materials used oil is grand celebration normal two wires distillate, and feedstock property is beneficial to table 1, and heat-eliminating medium is one of urine constituent Virahol, urine composition and reaction process condition as table 2 and table 3,
Described washing oil is boiling range is 120 ~ 160 DEG C of distillates, under complex reaction final temperature condition, washs complex compound.Then complex compound is heated to 60 ~ 70 DEG C and is decomposed into wax liquid and urine, and wax liquid anhydrates and washes, and urine loops back urine tank.Concrete outcome is in table 4.
Table 1 stock oil character
The table 2 Virahol urine aqueous solution forms
Table 3 reaction process condition
Table 4 embodiment result
Claims (9)
1. a Virahol urea aqueous solution by dewaxing method, it is characterized in that: enter reactor after stock oil and Virahol aqueous solution of urea mix and carry out complex reaction, described reactor operates at reduced pressure conditions, the vapor phase stream effluent of reactor head returns reactor through cooling Posterior circle, the reaction product part Returning reactor that reactor bottom obtains, remainder goes complex compound sedimentation washing tower to carry out later separation process, wherein, the feeding temperature of described reactor is 60 DEG C ~ 80 DEG C, reaction final temperature is 20 DEG C ~ 32 DEG C, and reactor operating pressure is 22 ~ 50kPa.
2. method according to claim 1, is characterized in that: reactor operating pressure is 30 ~ 40kPa.
3. method according to claim 1, is characterized in that: described stock oil and Virahol aqueous solution of urea feed weight are than being 1:5 ~ 1:30.
4. method according to claim 3, is characterized in that: described stock oil and Virahol aqueous solution of urea feed weight are than being 1:8 ~ 1:20.
5. method according to claim 1, is characterized in that: the vapor phase stream effluent of described reactor head enters tower reactor from the position of 2 ~ 6 different heights in the reactor lower part reactant bed of material along the tangential direction of reactor after cooling.
6. method according to claim 1, is characterized in that: the initial boiling point of described stock oil is 170 DEG C ~ 200 DEG C, and final boiling point is for being 320 DEG C ~ 350 DEG C.
7. method according to claim 6, is characterized in that: the feeding temperature of described reactor is 65 DEG C ~ 70 DEG C, and reaction final temperature is 25 DEG C ~ 30 DEG C.
8. method according to claim 1, is characterized in that: in described Virahol aqueous solution of urea, and urea concentration is 28wt% ~ 38wt%, and Virahol is 40wt% ~ 55wt%.
9. method according to claim 8, is characterized in that: in described Virahol aqueous solution of urea, and urea concentration is 30wt% ~ 35wt%, and Virahol is 46wt% ~ 50wt%.
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| CN105505357A (en) * | 2015-12-08 | 2016-04-20 | 中国石油天然气股份有限公司 | Chemical agent for improving quality of high-wax crude oil in situ and preparation method of chemical agent |
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| GB1373037A (en) * | 1972-02-17 | 1974-11-06 | Exxon Research Engineering Co | Continuous dewaxing oils in by -in situ- refrigeration |
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| CN103059999A (en) * | 2011-10-21 | 2013-04-24 | 中国石油化工股份有限公司 | Paraffin production method |
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2013
- 2013-10-24 CN CN201310503571.2A patent/CN104560195B/en active Active
Patent Citations (6)
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| GB1373037A (en) * | 1972-02-17 | 1974-11-06 | Exxon Research Engineering Co | Continuous dewaxing oils in by -in situ- refrigeration |
| CN1121104A (en) * | 1994-10-19 | 1996-04-24 | 中国石油化工总公司抚顺石油化工研究院 | Recovery method of dewaxing solvent for isopropanol urea |
| CN1151431A (en) * | 1995-11-30 | 1997-06-11 | 中国石油化工总公司抚顺石油化工研究院 | Method for reclaiming solvent in process of isopropyl alcohol urea |
| CN1218035A (en) * | 1997-11-24 | 1999-06-02 | 中国石油化工总公司 | Method for recovering solvent in dewaxing process of iospropyl alcohol urea |
| CN1733870A (en) * | 2004-08-12 | 2006-02-15 | 俞继亮 | Hydrosolvent urea dewaxing process for petroleum product |
| CN103059999A (en) * | 2011-10-21 | 2013-04-24 | 中国石油化工股份有限公司 | Paraffin production method |
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