CN103091475A - Method for determining petroleum distillate oil distillation range - Google Patents
Method for determining petroleum distillate oil distillation range Download PDFInfo
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- CN103091475A CN103091475A CN2011103325694A CN201110332569A CN103091475A CN 103091475 A CN103091475 A CN 103091475A CN 2011103325694 A CN2011103325694 A CN 2011103325694A CN 201110332569 A CN201110332569 A CN 201110332569A CN 103091475 A CN103091475 A CN 103091475A
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Abstract
The present invention provides a method for determining a petroleum distillate oil distillation range. According to the method, a vacuum distillation apparatus is adopted to carry out vacuum distillation on petroleum distillate oil to obtain distillates with different atmospheric equivalent temperatures, wherein the vacuum distillation apparatus comprises a vacuum unit and a distillation unit, the vacuum unit and the distillation unit are communicated through a pipeline, and the distillation unit comprises a distillation flask and a distillation column. The method comprises: conveying petroleum distillate oil into the distillation flask, and carrying out distillation on the distillation unit in the vacuum unit under a vacuum pumping condition, wherein a pressure in the distillation unit is 0.1-10 Pa, and the distillation flask and the distillation column form an integrated structure. With the method, heavy oil containing the distillate having an atmospheric equivalent temperature of more than 590 DEG C can be subjected to reduced pressure distillation so as to acquire distillation range data of the heavy oil. The method is particularly suitable for determination of distillation ranges of deep distillation wax oil and deep distillation residual oil.
Description
Technical field
The present invention relates to a kind of method of measuring the fraction oil of petroleum boiling range.
Background technology
At present, the cutting temperature of China's vacuum distillation apparatus vacuum residuum reaches as high as 540 ℃ of left and right, yet analyzes discovery by the composition to vacuum residuum, and vacuum residuum also contains potential petroleum refining raw material, as FCC raw material etc.Suitably improve and extract the yield that temperature can not only increase the crude oil light ends, reduce the output of the residual oil of low value, also can be for secondary processing provide more raw material, have great significance today in short supply at petroleum resources.
Therefore, be necessary vacuum residuum is carried out deep drawing (extracting temperature is 680 ℃ of left and right), light constituent residual in vacuum residuum is extracted, and the deep drawing wax oil (HVGO) that obtains and the composition of deep drawing residual oil (HVR) are analyzed, thereby provide rational suggestion for the processing of vacuum residuum.
Yet the analysis and characterization problem of HVGO and HVR is a great problem that the puzzlement researchist furthers investigate mink cell focus always, and one of them key issue is exactly how to obtain the boiling range data of HVGO and HVR.
ASTM D1160-06 provides a kind of petroleum products decompression distillation assay method, although the method can be carried out decompression distillation to heavy distillate, the highest normal pressure etc. of the sample that the method can be measured in theory is synthermal is 590 ℃.
Therefore, need badly and a kind ofly can obtain that to contain normal pressure etc. synthermal be the method for boiling range data of the sample of cut more than 590 ℃.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of method of measuring the fraction oil of petroleum boiling range is provided, the method can be that the mink cell focus of the cut more than 590 ℃ carries out decompression distillation to containing normal pressure etc. synthermal, and then obtains the boiling range data of these mink cell focuses.
the invention provides a kind of method of measuring the fraction oil of petroleum boiling range, the method uses a kind of vacuum distillation plant to carry out vacuum distillation to fraction oil of petroleum, obtain having the different synthermal cuts such as normal pressure, described vacuum distillation plant comprises vacuum unit and distills the unit, described vacuum unit and distillation are passed through pipeline connection between the unit, described distillation unit comprises cucurbit and distillation column, the method comprises to be sent into fraction oil of petroleum in described cucurbit, distill under the condition that described vacuum unit vacuumizes described distillation unit, wherein, pressure in described distillation unit is 0.1-10Pa, described cucurbit and described distillation column are structure as a whole.
Method of the present invention can be that the heavy distillate of cut more than 590 ℃ carries out decompression distillation to containing normal pressure etc. synthermal, and then obtains the boiling range data of these heavy distillates.Method of the present invention is specially adapted to the boiling range of deep drawing wax oil and deep drawing residual oil is measured.
Description of drawings
Accompanying drawing is to be used to provide a further understanding of the present invention, and consists of the part of instructions, is used from explanation the present invention with following embodiment one, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is used for cucurbit and the distillation column that explanation the method according to this invention is used;
Fig. 2 is used for the anti-return pipe of the distillation unit of explanation the method according to this invention;
Fig. 3 is used for a kind of embodiment of the distillation unit of explanation the method according to this invention;
Fig. 4 is used for the another kind of embodiment of the distillation unit of explanation the method according to this invention;
Fig. 5 is used for the vacuum cold trap that explanation the method according to this invention is used; And
Fig. 6 is used for the vacuum distillation plant that explanation the method according to this invention is used.
Embodiment
The invention provides a kind of method of measuring the fraction oil of petroleum boiling range, the method uses a kind of vacuum distillation plant to carry out vacuum distillation to fraction oil of petroleum, obtains having the different synthermal cuts such as normal pressure.
The method according to this invention, described vacuum distillation plant comprises vacuum unit and distills the unit, described vacuum unit and distillation are passed through pipeline connection between the unit, described distillation unit comprises cucurbit and distillation column, wherein, pressure in described distillation unit is 0.1-10Pa, and described cucurbit and described distillation column are structure as a whole.
In the present invention, the pressure in described distillation unit refer in cucurbit and distillation column and with other parts that cucurbit and distillation column communicate in pressure.Pressure in described distillation unit can be recorded by the conventional method of this area with absolute manometer.
According to the present invention, described vacuum unit comprises vacuum pump, and described vacuum pump is used for the distillation unit is vacuumized, and making the pressure in described distillation unit is 0.1-10Pa.
According to the present invention, described vacuum unit can adopt various vacuum pumps that the distillation unit is vacuumized, and makes within pressure in described distillation unit is in the scope of 0.1-10Pa.Of the present invention a kind of preferred embodiment in, can be by oil-sealed rotary pump and ODP be connected in series, and described oil-sealed rotary pump is vacuumized the distillation unit as the forepump of described ODP, make within pressure in described distillation unit is in the scope of 0.1-10Pa.The present invention is not particularly limited for the model of described oil-sealed rotary pump and described ODP, can be various oil-sealed rotary pumps and ODP commonly used.
According to the present invention, described vacuum unit can also comprise other element that this area is commonly used, and for example: described vacuum unit can also contain various operation valves for process control and for detection of the sensor of the pressure in the distillation unit.Said elements is known in the art, and those skilled in the art can carry out suitable selection according to concrete application scenario, and this paper repeats no more.
According to the present invention, described distillation unit comprises cucurbit and distillation column.The present inventor finds in practice process, reduces the pressure in vacuum distillation plant, needs to improve on the one hand the ability that vacuumizes of the vacuum pump in vacuum unit; Need on the other hand to improve the impermeability that vacuum distillation plant particularly distills the unit.Through deeply experiment, the present inventor finds, cucurbit and interface distillation column between of distillation in the unit is the bubble-tight principal element that affects vacuum distillation plant, by structure that cucurbit and distillation column are formed as one, can significantly improve the impermeability of vacuum distillation plant.Therefore, as shown in Figure 1, the distillation unit of the vacuum distillation plant that the method according to this invention is used comprises cucurbit 1 and distillation column 2, and described cucurbit 1 is structure as a whole with described distillation column 2.That is, according to the present invention, there is no interface between described cucurbit 1 and distillation column 2, and then eliminated under the condition of high temperature gas leak phenomenon that the existence due to interface produces.
According to the present invention, described distillation column 2 can for this area various distillation columns commonly used, be not particularly limited.Preferably, described distillation column 2 comprises vertical tube and the arm that stretches out from a side of described vertical tube, and described arm is downward-sloping.
In still-process, the steam that rises along described distillation column 2 is easy to condense on the vertical tube inwall of distillation column 2 and becomes drop, returns in cucurbit, has so not only reduced the efficient of distillation, has extended the time of distilling; And distillate is easy to occur cracking reaction owing to being heated for a long time.The present inventor finds in experimentation, if a back-flow preventer is set in distillation column 2, can play the effect of the amount that reduces phegma, shorten on the one hand the time of distillation, reduce on the other hand the probability of distillate generation heat scission reaction.The present invention is not particularly limited for described back-flow preventer, can be the various devices that can realize above-mentioned functions.
Of the present invention a kind of preferred embodiment in, as shown in Figure 2, described distillation column 2 also comprises the anti-return pipe 6 that is arranged in described vertical tube 4, the bottom outer wall of described anti-return pipe 6 and the inwall of described vertical tube 4 join, leave spacing between the top outer wall of described anti-return pipe 6 and the inwall of described vertical tube 4, be used for withdrawing fluid is guided in described arm 5.
This preferred embodiment is not particularly limited for the position of described anti-return pipe 6 in the vertical tube 4 of described distillation column 2, can carry out suitable selection according to the position of the arm 5 of described distillation column 2, is as the criterion withdrawing fluid can be guided in arm 5.
Preferably, the inwall of the bottom outer wall of described anti-return pipe 6 and described arm 5 engages at the inwall place of described vertical tube 4.Further preferably, the bottom that the inwall with described arm 5 of described anti-return pipe 6 engages to the ratio of the internal diameter of the minor increment of the top end face of described anti-return pipe 6 and described arm 5 is 0.1-0.5: 1, described minor increment is identical with the measurement unit of described internal diameter, can obtain higher distillation efficiency like this.
Of the present invention a kind of more preferred embodiment in, described anti-return pipe 6 is obliquely installed, and can make like this phegmas in described anti-return pipe 6 more steadily successfully enter in described arm 5.
In a kind of further preferred embodiment of the present invention, the bottom outer wall of described anti-return pipe 6 and the inwall of described arm 5 engage at the inwall place of described vertical tube 4, described anti-return pipe 6 is obliquely installed, and take surface level as benchmark, the angle of inclination of the bottom face of described anti-return pipe 6 is identical with the angle of inclination of the outline line of described arm 5.
Of the present invention a kind of further preferred embodiment in, the bottom outer wall of described anti-return pipe 6 and the inwall of described arm 5 engage at the inwall place of described vertical tube 4; Described anti-return pipe 6 is obliquely installed, and take surface level as benchmark, the angle of inclination of the bottom face of described anti-return pipe 6 is identical with the angle of inclination of the outline line of described arm 5; The bottom that the inwall with described arm 5 of described anti-return pipe 6 engages to the ratio of the internal diameter of the minor increment of the top end face of described anti-return pipe 6 and described arm 5 is 0.1-0.5: 1, and described minor increment is identical with the measurement unit of described internal diameter.
According to device of the present invention, described anti-return pipe 6 can have various shapes, as long as this anti-return pipe 6 can play, phegma is guided to the interior effect of described arm 5.For example, the cross section of described anti-return pipe 6 can be L shaped or splayed.Preferably, the cross section of described anti-return pipe 6 is splayed (as shown in Figure 2), can further improve like this ability of bearing high temperature of described anti-return pipe 6.From the angle of the ability of bearing high temperature of the described anti-return pipe 6 of further raising, the sidewall of described anti-return pipe 6 is splayed more preferably, and the sidewall of described anti-return pipe 6 has radian.
In a kind of most preferred embodiment of the present invention, as shown in Figure 2, the bottom outer wall of described anti-return pipe 6 and the inwall of described arm 5 engage at the inwall place of described vertical tube 4; Described anti-return pipe 6 is obliquely installed, and take surface level as benchmark, the angle of inclination of the bottom face of described anti-return pipe 6 is identical with the angle of inclination of the outline line of described arm 5; The bottom that inwall described anti-return pipe 6 and described arm 5 engages to the ratio of the internal diameter of the minor increment of the top end face of described anti-return pipe 6 and described arm 5 is 0.1-0.5: 1 (measurement unit of described minor increment and described internal diameter is identical); The cross section of described anti-return pipe 6 is splayed, and the sidewall of described anti-return pipe 6 has radian.
The present inventor finds in research process, the length that shortens distillation column 2 can shorten the vapor outlet port of distillation column 2 and the distance between the distillate in cucurbit 1, thereby be conducive to steaming of the interior distillate of cucurbit 1, the efficient according to device of the present invention can be further improved on the one hand, the probability that cracking reaction at high temperature occurs distillate can be further reduced on the other hand.Therefore, of the present invention a kind of preferred embodiment in, the volume of described cucurbit 1 is the 0.1-1 liter, the length of described distillation column 2 (that is, is pushed up to distillate from cucurbit and is distillated column length between the position; Also namely, from the column length between position to the lower edge of the arm of distillation column that cucurbit and distillation column intersect) be 10-50mm.The length of described distillation column 2 is 30-45mm more preferably.
The method according to this invention, as shown in Figure 1, described distillation column 2 preferably has insulation jacket 3, described insulation jacket 3 is kept apart outer wall and the external environment of distillation column 2, can play the effect of insulation, further reduce the phenomenon that steam condensing refluxes, and then can further shorten the time of vacuum distillation.Described insulation jacket can for this area various insulation jacket that can realize above-mentioned functions commonly used, be not particularly limited.
According to the present invention, the distillation unit of described vacuum distillation plant preferably has the stirring apparatus that stirs for to the distillate in described cucurbit 1, like this can be so that in still-process, and distillate is heated evenly.According to the present invention, described stirring apparatus is preferably magnetic agitation, can make distillate be heated evenly so on the one hand, also can the impermeability of distilling the unit not had a negative impact on the other hand.
The method according to this invention, described distillation unit can also comprise for the temperature sensor of measuring steam temperature and distillate temperature.The present invention is not particularly limited for kind and the installation site of described temperature sensor, can select for the routine of this area.For example, can be by temperature sensor be inserted into lower to concordant with the arm 5 of described distillation column 2 from the interface on the vertical tube 4 of described distillation column 2, thus detect steam temperature.Again for example, during distillate temperature in measuring cucurbit, can temperature sensor be inserted in distillate by this interface by on described cucurbit 1, interface being set, thereby detect the distillate temperature.Bubble-tight angle from the described vacuum distillation plant of further raising, in the distillation unit of described vacuum distillation plant, preferred employing can detect the double temperature sensor of the temperature of two positions simultaneously, detects simultaneously distillate temperature in cucurbit 1 and 5 times steam temperatures along the place of arm of distillation column 2.
According to the present invention, described distillation unit can also contain normally used other parts in still-process, and for example: condenser, distillate receiver and well heater, this paper repeats no more.
Fig. 3 shows a kind of embodiment of the distillation unit of the vacuum distillation plant that uses in method of the present invention.According to this embodiment, described distillation unit comprises cucurbit 1, distillation column 2, insulation jacket 3, is positioned at the stirring magneton 7 of described cucurbit 1, the double temperature sensor 8 that can measure simultaneously distillate temperature and steam temperature, magnetic stirring apparatus 9, upper heating jacket 10, lower heating jacket 11, condenser pipe 12 and receive graduated cylinder 13, wherein, described cucurbit 1 is structure as a whole with distillation column 2, is provided with previously described anti-return pipe (not shown) in the vertical tube of described distillation column 2.
Fig. 4 shows the another kind of embodiment of the distillation unit of the vacuum distillation plant that uses in method of the present invention.In this embodiment, be provided with temperature sensor interface above the side of cucurbit 1, temperature sensor 14 stretches in the interior distillate of cucurbit 1 by this interface, for detection of described distillate temperature, temperature sensor 15 stretches in described distillation column 2 by the interface on the vertical tube of distillation column 2, concordant with the lower edge of the arm of distillation column 2, to detect steam temperature.
According to the present invention, on pipeline between described vacuum unit and described distillation unit, vacuum cold trap is set preferably, to capture the condensability oil gas from the air-flow of described distillation unit extraction, can further reduce on the one hand the pressure in vacuum distillation plant, can prevent from the other hand coming from the vacuum pump that the oil gas that distills the unit enters described vacuum unit, shorten the serviceable life of vacuum pump and reduce the work efficiency of vacuum pump.
According to the present invention, described vacuum distillation plant is not particularly limited for described vacuum cold trap, can select for the routine of this area.According to the present invention, described vacuum cold trap can make vacuum cold trap remain low temperature by the method with cooling liquid, to capture from the condensability oil gas in the air-flow of described distillation unit.
The present invention is not particularly limited for the kind of described cooling liquid, can be various cooling liquids commonly used, for example: liquid nitrogen.The present invention also is not particularly limited for the temperature of described liquid coolant, as long as the temperature sufficient to guarantee of described liquid coolant can be with the condensability oil gas condensation.Preferably, the temperature of described liquid coolant is-120 ℃ to-60 ℃.
The present invention also is not particularly limited for the structure of described vacuum cold trap, can select for the routine of this area.For example, the vacuum trap body of described vacuum cold trap can be the U font, the space that the vacuum trap body surrounds can be used for holding liquid coolant, the gas access that is oppositely arranged on the sidewall of described vacuum trap body and gas vent, wherein, described gas access is connected with described distillation unit, and described gas vent is connected with described vacuum unit.Again for example, the vacuum trap body of described vacuum cold trap can be the cup type, and the gas access can be arranged on the top cover of described vacuum trap body; Gas vent both can be arranged on the top cover of described vacuum trap body, also can be arranged on the sidewall of described vacuum trap body, during use, described vacuum cold trap was placed in liquid coolant and got final product.
The present inventor is in research process, although between described vacuum unit and described distillation unit, the amount that vacuum cold trap can reduce the condensable gas that enters described vacuum unit is set, but the synthermal height such as normal pressure of and the cut that distillate low due to the pressure in the distillation unit of the method according to this invention, thereby the content of the condensability oil gas in the air-flow that aspirates out from distill the unit is also higher, be easy to be sucked in the cavity of vacuum pump, and then shorten the serviceable life of vacuum pump.
The present inventor finds by great many of experiments, by in the vacuum trap body of described vacuum cold trap, a mozzle being set, guiding enters in the vacuum trap body from the inwall that the air-flow of described distillation unit contacts with liquid coolant along described vacuum trap body, make like this air-flow can contact with the cooling wall of vacuum cold trap once entering the vacuum trap body, thereby further improve the cooling effectiveness of vacuum cold trap.
of the present invention a kind of preferred embodiment in, as shown in Figure 5, described vacuum cold trap comprises that the cross section is the vacuum trap body 18 of U font, be nested in the mozzle 16 in described vacuum trap body, gas access 19-1 and gas vent 19-2, described mozzle 16 is hanging connected in the top of described vacuum trap body 18 and leaves spacing with the both sides inwall of described vacuum trap body 18, the bottom opening of described mozzle 16 and leave spacing with the bottom interior wall of described vacuum trap body 18, the sidewall that described gas access 19-1 passes vacuum trap body 18 is arranged on described mozzle 16, described gas vent 19-2 is arranged on the sidewall of described vacuum trap body 18, make air-flow leave described vacuum trap body 18 along the outer wall of described mozzle 16.
The method according to this invention is not particularly limited for the pipeline that connects described distillation unit and described vacuum unit, can select for this area is conventional, and this paper repeats no more.
Fig. 6 shows a kind of arrangement of the vacuum distillation plant that uses in method of the present invention.As shown in Figure 6, vacuum unit adopts oil-sealed rotary pump and the ODP that is connected in series, and wherein oil-sealed rotary pump is as the forepump of described ODP, and during work, at first the temperature with vacuum cold trap is reduced to below-70 ℃; Then start oil-sealed rotary pump, open manual vacuum switch valve 20,21 and 22, making the cavity of ODP and the pressure of distillation in the unit is below 100Pa; Then close manual vacuum switch valve 21, and start ODP and automatically control vacuum solenoid 23, the unlatching ratio of regulating described automatic control vacuum solenoid 23 according to the pressure in predetermined distillation unit; When the pressure in the vacuum distilling apparatus is in 0.1-10Pa, cucurbit is heated, and control the degree of heat of heating arrangement, make the interior distillate of cucurbit heat up with the speed of 6-8 ℃/min; After having distillate to distillate, the degree of controlling heating makes distillate distillate with the speed of 5-10mL/min.
The method according to this invention comprises to be sent into fraction oil of petroleum in described cucurbit, distills under the condition that described vacuum unit vacuumizes described distillation unit, and receives respectively the cut with different recovered (distilled) temperatures with the cut receiver.Particularly, described fraction oil of petroleum is sent in described cucurbit, carrying out vacuum distillation measures the mode of its boiling range and comprises: fraction oil of petroleum is put into cucurbit, open vacuum unit, make distillation unit internal pressure reach 0.1-10Pa, the heating cucurbit, the distillate of collection initial boiling point, each distillation yield cut and the end point of distillation.Described each distillation yield cut preferably includes percent by volume and is respectively 5%, 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90% and 95% distillate.Described distillation yield percentage is the percent by volume of distillate and distillation.Record steam temperature and pressure that each cut distillates during distillation, steam temperature is converted into the synthermal boiling ranges that namely obtain this fraction oil of petroleum such as normal pressure.Can adopting this area the whole bag of tricks commonly used that described steam temperature is converted, to become the normal pressure of this cut etc. synthermal, and the present invention becomes normal pressure etc. synthermal by the distillation conversion pressure steam temperature observed in still-process by table 1.In addition, for the steam temperature that does not provide in table 1, it is synthermal that the formula that provides in can the appendix A 7 by method of interpolation or ASTM D1160-06 is converted into normal pressure etc.That the formula that provides in the appendix A 7 by ASTM D1160-06 converts in the embodiment of the present invention.
Table 1
The method according to this invention, described fraction oil of petroleum can be the fraction oil of petroleum in various sources.Preferably, described fraction oil of petroleum is for by carrying out to long residuum or vacuum residuum deep drawing wax oil and/or the deep drawing residual oil that deep drawing obtains.
With method of the present invention to fraction oil of petroleum (particularly deep drawing wax oil or deep drawing wax oil) when carrying out decompression distillation, the cut that distillates can comprise the synthermal cut for 540-720 ℃ such as normal pressure.
Describe the present invention in detail below in conjunction with embodiment.
Embodiment 1-10 is used for illustrating the method according to mensuration fraction oil of petroleum boiling range of the present invention.
Adopt device shown in Figure 6, wherein, the distillation unit as shown in Figure 3, distillation column length is 35mm, distillation column as shown in Figure 2, the anti-return pipe is inclined in the vertical tube of distillation column, and take surface level as benchmark, the angle of inclination of the bottom face of described anti-return pipe is identical with the angle of inclination of the outline line of described arm; The bottom outer wall of described anti-return pipe and the inwall of described arm engage at the inwall place of described vertical tube, and the bottom that engages with inwall described arm described anti-return pipe to the ratio of the internal diameter of the minor increment of the top end face of described anti-return pipe and described arm is 0.5; Adopt vacuum cold trap shown in Figure 5.
91.85 No. 2 deep drawing wax oils of gram Chad are placed in the cucurbit of 500mL, then carry out vacuum distillation according to following flow process.
The temperature of vacuum cold trap is reduced to-70 ℃; Then start oil-sealed rotary pump, open manual vacuum switch valve 20,21 and 22, making the cavity of ODP and the pressure of distillation in the unit is 100Pa; Then close manual vacuum switch valve 21, and start ODP and automatically control vacuum solenoid 23; When the pressure in distilling the unit is 0.1Pa, cucurbit is heated, and control the degree of heat of heating arrangement, make the interior distillate of cucurbit heat up with the speed of 6 ℃/min; After having distillate to distillate, the degree of controlling heating makes distillate distillate with the speed of 5mL/min, steam temperature and pressure when recording each cut in still-process and distillating.
The steam temperature that obtains is converted into normal pressure etc. by table 1 synthermal, obtains the boiling range data of No. 2 deep drawing wax oils of Chad, result is shown in table 2.
Table 2
| Distillation yield (volume %) | Normal pressure etc. synthermal (℃) |
| Initial boiling point | 511 |
| 5 | 563 |
| 10 | 572 |
| 20 | 588 |
| 30 | 601 |
| 40 | 612 |
| 50 | 621 |
| 60 | 629 |
| 70 | 636 |
| 80 | 642 |
| 90 | 647 |
| 95 | 649 |
Adopt device shown in Figure 6, wherein, the distillation unit as shown in Figure 3, distillation column length is 35mm, distillation column as shown in Figure 2, the anti-return pipe is inclined in the vertical tube of distillation column, and take surface level as benchmark, the angle of inclination of the bottom face of described anti-return pipe is identical with the angle of inclination of the outline line of described arm; The bottom outer wall of described anti-return pipe and the inwall of described arm engage at the inwall place of described vertical tube, and the bottom that engages with inwall described arm described anti-return pipe to the ratio of the internal diameter of the minor increment of the top end face of described anti-return pipe and described arm is 0.1; Adopt vacuum cold trap shown in Figure 5.
90.09 gram Ackers are entangled the cucurbit that guest's deep drawing wax oil is placed in 500mL, then carry out vacuum distillation according to following flow process.
At first the temperature with vacuum cold trap is reduced to-75 ℃; Then start oil-sealed rotary pump, open manual vacuum switch valve 20,21 and 22, making the cavity of ODP and the pressure of distillation in the unit is 90Pa; Then close manual vacuum switch valve 21, and start ODP and automatically control vacuum solenoid 23; When the pressure in distilling the unit is 1Pa, cucurbit is heated, and control the degree of heat of heating arrangement, make the interior distillate of cucurbit heat up with the speed of 7 ℃/min; After having distillate to distillate, the degree of controlling heating makes distillate distillate with the speed of 8mL/min, steam temperature and pressure when recording each cut in still-process and distillating.
The steam temperature that obtains is converted into normal pressure etc. by table 1 synthermal, obtains the boiling range data that Acker entangles guest's deep drawing wax oil, result is shown in table 3.
Table 3
| Distillation yield (volume %) | Normal pressure etc. synthermal (℃) |
| Initial boiling point | 523 |
| 5 | 548 |
| 10 | 555 |
| 20 | 570 |
| 30 | 584 |
| 40 | 597 |
| 50 | 609 |
| 60 | 620 |
| 70 | 630 |
| 80 | 639 |
| 90 | 646 |
| 95 | 650 |
Adopt device shown in Figure 6, wherein, the distillation unit as shown in Figure 3, distillation column length is 45mm, distillation column as shown in Figure 2, the anti-return pipe is inclined in the vertical tube of distillation column, and take surface level as benchmark, the angle of inclination of the bottom face of described anti-return pipe is identical with the angle of inclination of the outline line of described arm; The bottom outer wall of described anti-return pipe and the inwall of described arm engage at the inwall place of described vertical tube, and the bottom that engages with inwall described arm described anti-return pipe to the ratio of the internal diameter of the minor increment of the top end face of described anti-return pipe and described arm is 0.3; Adopt vacuum cold trap shown in Figure 5.
90.50 gram instrument long lines deep drawing wax oils are placed in the cucurbit of 500mL, then carry out vacuum distillation according to following flow process.
At first the temperature with vacuum cold trap is reduced to-90 ℃; Then start oil-sealed rotary pump, open manual vacuum switch valve 20,21 and 22, making the cavity of ODP and the pressure of distillation in the unit is 80Pa; Then close manual vacuum switch valve 21, and start ODP and automatically control vacuum solenoid 23; When the pressure in distilling the unit is 10Pa, cucurbit is heated, and control the degree of heat of heating arrangement, make the interior distillate of cucurbit heat up with the speed of 8 ℃/min; After having distillate to distillate, the degree of controlling heating makes distillate distillate with the speed of 10mL/min, steam temperature and pressure when recording each cut in still-process and distillating.
The steam temperature that obtains is converted into normal pressure etc. by table 1 synthermal, obtains the boiling range data of instrument long lines deep drawing wax oil, result is shown in table 4.
Table 4
| Distillation yield (volume %) | Normal pressure etc. synthermal (℃) |
| Initial boiling point | 342 |
| 5 | 438 |
| 10 | 475 |
| 20 | 534 |
| 30 | 573 |
| 40 | 598 |
| 50 | 613 |
| 60 | 621 |
| 70 | 628 |
| 80 | 636 |
| 90 | 651 |
| 95 | 662 |
Adopt the method identical with embodiment 1 to carry out vacuum distillation to card human relations deep drawing wax oil, the boiling range data that obtain are shown in table 5.
Table 5
| Distillation yield (volume %) | Normal pressure etc. synthermal (℃) |
| Initial boiling point | 476 |
| 5 | 540 |
| 10 | 549 |
| 20 | 565 |
| 30 | 580 |
| 40 | 593 |
| 50 | 605 |
| 60 | 616 |
| 70 | 627 |
| 80 | 638 |
| 90 | 648 |
| 95 | 654 |
Adopt the method identical with embodiment 3 to carry out vacuum distillation to DOPA deep drawing wax oil, the boiling range data that obtain are shown in table 6.
Table 6
| Distillation yield (volume %) | Normal pressure etc. synthermal (℃) |
| Initial boiling point | 479 |
| 5 | 548 |
| 10 | 561 |
| 20 | 584 |
| 30 | 600 |
| 40 | 613 |
| 50 | 623 |
| 60 | 631 |
| 70 | 640 |
| 80 | 651 |
| 90 | 665 |
| 95 | 674 |
Adopt the method identical with embodiment 1 to carry out vacuum distillation to Kuwait's deep drawing wax oil, the boiling range data that obtain are shown in table 7.
Table 7
| Distillation yield (volume %) | Normal pressure etc. synthermal (℃) |
| Initial boiling point | 472 |
| 5 | 545 |
| 10 | 556 |
| 20 | 576 |
| 30 | 592 |
| 40 | 606 |
| 50 | 618 |
| 60 | 628 |
| 70 | 637 |
| 80 | 645 |
| 90 | 653 |
| 95 | 657 |
Embodiment 7
Adopt the method identical with embodiment 1 to carry out vacuum distillation to A Muna deep drawing wax oil, the boiling range data that obtain are shown in table 8.
Table 8
| Distillation yield (volume %) | Normal pressure etc. synthermal (℃) |
| Initial boiling point | 469 |
| 5 | 558 |
| 10 | 567 |
| 20 | 583 |
| 30 | 596 |
| 40 | 608 |
| 50 | 618 |
| 60 | 627 |
| 70 | 635 |
| 80 | 642 |
| 90 | 649 |
| 95 | 653 |
Embodiment 8
Adopt the method identical with embodiment 1 to carry out vacuum distillation to grand celebration deep drawing wax oil, the boiling range data that obtain are shown in table 9.
Table 9
| Distillation yield (volume %) | Normal pressure etc. synthermal (℃) |
| Initial boiling point | 437 |
| 5 | 535 |
| 10 | 548 |
| 20 | 568 |
| 30 | 582 |
| 40 | 593 |
| 50 | 600 |
| 60 | 607 |
| 70 | 616 |
| 80 | 627 |
| 90 | 643 |
| 95 | 653 |
Adopt the method identical with embodiment 1 to the Asia, Witter hereby the deep drawing wax oil carry out vacuum distillation, the boiling range data that obtain are shown in table 10.
Table 10
| Distillation yield (volume %) | Normal pressure etc. synthermal (℃) |
| Initial boiling point | 458 |
| 5 | 534 |
| 10 | 543 |
| 20 | 559 |
| 30 | 573 |
| 40 | 586 |
| 50 | 598 |
| 60 | 609 |
| 70 | 620 |
| 80 | 631 |
| 90 | 643 |
| 95 | 649 |
Adopt device shown in Figure 6, wherein, the distillation unit as shown in Figure 4, distillation column length is 35mm, distillation column as shown in Figure 2, the anti-return pipe is inclined in the vertical tube of distillation column, and take surface level as benchmark, the angle of inclination of the bottom face of described anti-return pipe is identical with the angle of inclination of the outline line of described arm; The bottom outer wall of described anti-return pipe and the inwall of described arm engage at the inwall place of described vertical tube, and the bottom that engages with inwall described arm described anti-return pipe to the ratio of the internal diameter of the minor increment of the top end face of described anti-return pipe and described arm is 0.3; Adopt the vacuum cold trap identical with vacuum cold trap shown in Figure 5, in the vacuum trap body of different is vacuum cold trap, mozzle is not set.
90.51 gram Tarim Basin deep drawing wax oils are placed in the cucurbit of 500mL, then carry out vacuum distillation according to following flow process.
The temperature of vacuum cold trap is reduced to-70 ℃; Then start oil-sealed rotary pump, open manual vacuum switch valve 20,21 and 22, making the cavity of ODP and the pressure of distillation in the unit is 100Pa; Then close manual vacuum switch valve 21, and start ODP and automatically control vacuum solenoid 23; When the pressure in distilling the unit is 10Pa, cucurbit is heated, and control the degree of heat of heating arrangement, make the interior distillate of cucurbit heat up with the speed of 7 ℃/min; After having distillate to distillate, the degree of controlling heating makes distillate distillate with the speed of 5mL/min, steam temperature and pressure when recording each cut in still-process and distillating.
The steam temperature that obtains is converted into normal pressure etc. by table 1 synthermal, obtains the boiling range data of Tarim Basin deep drawing wax oil, result is shown in table 11.
Table 11
| Distillation yield (volume %) | Normal pressure etc. synthermal (℃) |
| Initial boiling point | 471 |
| 5 | 530 |
| 10 | 538 |
| 20 | 552 |
| 30 | 565 |
| 40 | 577 |
| 50 | 588 |
| 60 | 600 |
| 70 | 611 |
| 80 | 623 |
| 90 | 635 |
| 95 | 642 |
The result of embodiment 1-10 shows, the method according to this invention is can be to the normal pressure of cut etc. synthermal is that fraction oil of petroleum more than 590 ℃ carries out decompression distillation, and then obtains the boiling range data of this fraction oil of petroleum.
Claims (16)
1. method of measuring the fraction oil of petroleum boiling range, the method uses a kind of vacuum distillation plant to carry out vacuum distillation to fraction oil of petroleum, obtain having the different synthermal cuts such as normal pressure, described vacuum distillation plant comprises vacuum unit and distills the unit, described vacuum unit and distillation are passed through pipeline connection between the unit, described distillation unit comprises cucurbit and distillation column, the method comprises to be sent into fraction oil of petroleum in described cucurbit, distill under the condition that described vacuum unit vacuumizes described distillation unit, it is characterized in that, pressure in described distillation unit is 0.1-10Pa, described cucurbit and described distillation column are structure as a whole.
2. method according to claim 1, wherein, the vacuum pump in described vacuum unit comprises oil-sealed rotary pump and the ODP that is connected in series, described oil-sealed rotary pump is as the forepump of described ODP.
3. method according to claim 1, wherein, the volume of described cucurbit is the 0.1-1 liter, the length of described distillation column is 10-50mm.
4. method according to claim 1, wherein, described distillation column has insulation jacket.
5. the described method of any one according to claim 1,3 and 4, wherein, described distillation column comprises vertical tube and the arm that stretches out from a side of described vertical tube, described arm is downward-sloping.
6. method according to claim 5, wherein, described distillation column also comprises the anti-return pipe that is arranged in described vertical tube, the bottom outer wall of described anti-return pipe and the inwall of described vertical tube join, leave spacing between the top outer wall of described anti-return pipe and the inwall of described vertical tube, be used for withdrawing fluid is guided in described arm.
7. method according to claim 6, wherein, the bottom outer wall of described anti-return pipe and the inwall of described arm engage at the inwall place of described vertical tube.
8. method according to claim 7, wherein, described anti-return pipe is obliquely installed.
9. method according to claim 8, wherein, take surface level as benchmark, the angle of inclination of the bottom face of described anti-return pipe is identical with the angle of inclination of the outline line of described arm.
10. method according to claim 7, wherein, the bottom that engages with inwall described arm described anti-return pipe to the ratio of the internal diameter of the minor increment of the top end face of described anti-return pipe and described arm is 0.1-0.5: 1.
11. method according to claim 6, wherein, the cross section of described anti-return pipe is splayed.
12. method according to claim 1 wherein, is provided with vacuum cold trap on the pipeline between described distillation unit and described vacuum unit.
13. method according to claim 12, wherein, described vacuum cold trap comprises that the cross section is the vacuum trap body of U font, be nested in the mozzle in described vacuum trap body, gas access and gas vent, described mozzle is hanging connected in the top of described vacuum trap body and leaves spacing with the both sides inwall of described vacuum trap body, the bottom opening of described mozzle and leave spacing with the bottom interior wall of described vacuum trap body, the sidewall that described vacuum trap body is passed in described gas access is arranged on described mozzle, described gas vent is arranged on the sidewall of described vacuum trap body, make air-flow leave described vacuum trap body along the outer wall of described mozzle.
14. method according to claim 1, wherein, using described vacuum distillation plant to carry out vacuum distillation to fraction oil of petroleum measures the mode of its boiling range and comprises: fraction oil of petroleum is put into cucurbit, open vacuum unit, make distillation unit internal pressure reach 0.1-10Pa, the heating cucurbit, the distillate of collection initial boiling point, each distillation yield cut and the end point of distillation.
15. according to claim 1 or 14 described methods, wherein, described cut comprises the synthermal cut for 540-720 ℃ such as normal pressure.
16. according to claim 1 or 14 described methods, wherein, described fraction oil of petroleum is deep drawing wax oil and/or deep drawing residual oil.
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| CN105388085A (en) * | 2015-12-22 | 2016-03-09 | 陈国庆 | Device and technological method for detecting distillation range of crude oil through mass method |
| CN105675645A (en) * | 2016-03-02 | 2016-06-15 | 南京理工大学 | Backflow preventing part for adiabatic calorimeter |
| CN107255706A (en) * | 2017-07-07 | 2017-10-17 | 四川西普石油物资装备有限公司 | Prevent occurring the method for rushing sample when crude oil from determining |
| CN109839495A (en) * | 2019-03-22 | 2019-06-04 | 杭州辛孚能源科技有限公司 | A method of light petroleum fraction boiling range is calculated according to molecular composition |
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| CN109839495A (en) * | 2019-03-22 | 2019-06-04 | 杭州辛孚能源科技有限公司 | A method of light petroleum fraction boiling range is calculated according to molecular composition |
| CN109839495B (en) * | 2019-03-22 | 2021-07-23 | 广东辛孚科技有限公司 | Method for calculating distillation range of light petroleum fraction according to molecular composition |
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