CN103091475B - A kind of method measuring fraction oil of petroleum boiling range - Google Patents
A kind of method measuring fraction oil of petroleum boiling range Download PDFInfo
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- CN103091475B CN103091475B CN201110332569.4A CN201110332569A CN103091475B CN 103091475 B CN103091475 B CN 103091475B CN 201110332569 A CN201110332569 A CN 201110332569A CN 103091475 B CN103091475 B CN 103091475B
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Abstract
The invention provides a kind of method measuring 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 that there is the synthermal cuts such as different normal pressures, described vacuum distillation plant comprises vacuum unit and distillation unit, pipeline connection is passed through between described vacuum unit and distillation unit, described distillation unit comprises cucurbit and distillation column, the method comprises to be sent in described cucurbit by fraction oil of petroleum, distill under the condition that described vacuum unit vacuumizes described distillation unit, 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 to containing normal pressure etc. synthermal be that the mink cell focus of more than 590 DEG C cuts carries out decompression distillation, and then obtain the boiling range data of these mink cell focuses.Method of the present invention is specially adapted to measure the boiling range of deep drawing wax oil and deep drawing residual oil.
Description
Technical field
The present invention relates to a kind of method measuring 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 about 540 DEG C, but finds by carrying out analysis to the composition of vacuum residuum, and vacuum residuum also contains potential petroleum refining raw material, as FCC raw material etc.The yield that temperature can not only increase crude oil light ends is extracted in suitable raising, reduces the output of the residual oil of low value, also can provide more raw material for secondary processing, have great significance in today that petroleum resources are in short supply.
Therefore, be necessary to carry out deep drawing (extracting temperature is about 680 DEG C) to vacuum residuum, the light constituent remained in vacuum residuum is extracted, and the composition of the deep drawing wax oil (HVGO) obtained and deep drawing residual oil (HVR) is analyzed, thus provide rational suggestion for the processing of vacuum residuum.
But the analysis and characterization problem of HVGO and HVR is a great problem that puzzlement researchist furthers investigate mink cell focus, and one of them key issue is exactly the boiling range data how obtaining HVGO and HVR always.
ASTMD1160-06 provides a kind of petroleum products decompression distillation assay method, although the method can carry out decompression distillation to heavy distillate, the sample that the method can measure in theory the highest normal pressure etc. is synthermal is 590 DEG C.
Therefore, need badly a kind of can obtain containing normal pressure etc. synthermal be the method for the boiling range data of the sample of more than 590 DEG C cuts.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of method measuring fraction oil of petroleum boiling range is provided, the method can to containing normal pressure etc. synthermal be that the mink cell focus of the cut of more than 590 DEG C carries out decompression distillation, and then obtain the boiling range data of these mink cell focuses.
The invention provides a kind of method measuring 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 that there is the synthermal cuts such as different normal pressures, described vacuum distillation plant comprises vacuum unit and distillation unit, pipeline connection is passed through between described vacuum unit and distillation unit, described distillation unit comprises cucurbit and distillation column, the method comprises to be sent in described cucurbit by fraction oil of petroleum, 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 to containing normal pressure etc. synthermal be that the heavy distillate of more than 590 DEG C cuts carries out decompression distillation, and then obtain the boiling range data of these heavy distillates.Method of the present invention is specially adapted to measure the boiling range of deep drawing wax oil and deep drawing residual oil.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and forms a part for instructions, is used from explanation the present invention, but is not construed as limiting the invention with embodiment one below.In the accompanying drawings:
The cucurbit that Fig. 1 uses for illustration of method according to the present invention and distillation column;
Fig. 2 is for illustration of the anti-return pipe in the distillation unit of method according to the present invention;
Fig. 3 is for illustration of a kind of embodiment of the distillation unit of method according to the present invention;
Fig. 4 is for illustration of the another kind of embodiment of the distillation unit of method according to the present invention;
The vacuum cold trap that Fig. 5 uses for illustration of method according to the present invention; And
The vacuum distillation plant that Fig. 6 uses for illustration of method according to the present invention.
Embodiment
The invention provides a kind of method measuring 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 synthermal cuts such as different normal pressures.
According to method of the present invention, described vacuum distillation plant comprises vacuum unit and distillation unit, pipeline connection is passed through between described vacuum unit and distillation 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 refers to cucurbit and the pressure in distillation column and in other parts communicated with cucurbit and distillation column.Pressure in described distillation unit, with absolute manometer, can be recorded by the conventional method of this area.
According to the present invention, described vacuum unit comprises vacuum pump, and described vacuum pump is used for vacuumizing distillation unit, makes the pressure in described distillation unit be 0.1-10Pa.
According to the present invention, described vacuum unit can adopt various vacuum pump to vacuumize distillation unit, and the pressure in described distillation unit is within the scope of 0.1-10Pa.One of the present invention preferred embodiment in, can by oil-sealed rotary pump and ODP be connected in series, and the forepump of described oil-sealed rotary pump as described ODP is vacuumized distillation unit, the pressure in described distillation unit is within 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 conventional various oil-sealed rotary pump and ODP.
According to the present invention, described vacuum unit can also comprise other conventional element of this area, such as: described vacuum unit can also containing the various operation valve for process control and the sensor for detecting the pressure in 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, repeat no more herein.
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 the ability vacuumized of the vacuum pump improved in vacuum unit on the one hand; Then need on the other hand to improve the impermeability that vacuum distillation plant particularly distills unit.Through deeply experiment, the present inventor finds, cucurbit in distillation unit and the interface between distillation column are the bubble-tight principal elements affecting vacuum distillation plant, by the structure that cucurbit and distillation column 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 method according to the present invention uses comprises cucurbit 1 and distillation column 2, and described cucurbit 1 and described distillation column 2 are structure as a whole.That is, according to the present invention, between described cucurbit 1 and distillation column 2, interface is not had, and then the gas leak phenomenon produced due to the existence of interface under eliminating the condition of high temperature.
According to the present invention, the various distillation columns that described distillation column 2 can be commonly used for this area, are not particularly limited.Preferably, the arm that described distillation column 2 comprises vertical tube and stretches out from the side of described vertical tube, described arm is downward-sloping.
In still-process, the steam risen along described distillation column 2 is easy to become drop at the vertical tube condensed on inner walls of distillation column 2, returns in cucurbit, not only reduces the efficiency of distillation like this, extend the time of distillation; And distillate is easy to owing to being heated for a long time cracking reaction occurs.The present inventor finds in experimentation, if arrange a back-flow preventer in distillation column 2, then can play the effect of the amount reducing phegma, shorten the time of distillation on the one hand, then reduce the probability of distillate generation heat scission reaction on the other hand.The present invention is not particularly limited for described back-flow preventer, can be the various device that can realize above-mentioned functions.
One of the present invention preferred embodiment in, as shown in Figure 2, described distillation column 2 also comprises the anti-return pipe 6 be arranged in described vertical tube 4, the bottom outer wall of described anti-return pipe 6 connects with the inwall of described vertical tube 4, spacing is left, for being guided to by withdrawing fluid in described arm 5 between the top outer wall of described anti-return pipe 6 and the inwall of described vertical tube 4.
This is preferred embodiment 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 bottom outer wall of described anti-return pipe 6 engages at the inwall place of described vertical tube 4 with the inwall of described arm 5.Further preferably, the bottom engaged with the inwall of described arm 5 of described anti-return pipe 6 is 0.1-0.5: 1 to the minor increment of top end face of described anti-return pipe 6 and the ratio of the internal diameter of described arm 5, described minor increment is identical with the measurement unit of described internal diameter, can obtain higher distillation efficiency like this.
One of the present invention more preferred embodiment in, described anti-return pipe 6 is obliquely installed, and can make that the phegma in described anti-return pipe 6 is more steady successfully to be entered in described arm 5 like this.
In a kind of further preferred embodiment of the present invention, the bottom outer wall of described anti-return pipe 6 engages at the inwall place of described vertical tube 4 with the inwall of described arm 5, described anti-return pipe 6 is obliquely installed, and be benchmark with surface level, 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.
One of the present invention further preferred embodiment in, the bottom outer wall of described anti-return pipe 6 engages at the inwall place of described vertical tube 4 with the inwall of described arm 5; Described anti-return pipe 6 is obliquely installed, and is benchmark with surface level, and 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 engaged with the inwall of described arm 5 of described anti-return pipe 6 is 0.1-0.5: 1 to the minor increment of top end face of described anti-return pipe 6 and the ratio of the internal diameter of described arm 5, 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 shape, as long as this anti-return pipe 6 can play the effect guided to by phegma in described arm 5.Such as, the cross section of described anti-return pipe 6 can be L shape or splayed.Preferably, the cross section of described anti-return pipe 6 is splayed (as shown in Figure 2), can improve the ability of bearing high temperature of described anti-return pipe 6 so further.From the angle of bearing the ability of high temperature improving described anti-return pipe 6 further, the sidewall of described anti-return pipe 6 is more preferably splayed, and the sidewall of described anti-return pipe 6 has radian.
In the most preferred embodiment of one of the present invention, as shown in Figure 2, the bottom outer wall of described anti-return pipe 6 engages at the inwall place of described vertical tube 4 with the inwall of described arm 5; Described anti-return pipe 6 is obliquely installed, and is benchmark with surface level, and 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 engaged with the inwall of described arm 5 of described anti-return pipe 6 is 0.1-0.5: 1 (measurement unit of described minor increment and described internal diameter is identical) to the minor increment of top end face of described anti-return pipe 6 and the ratio of the internal diameter of described arm 5; 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, shorten the distance between distillate that the length of distillation column 2 can shorten in the vapor outlet port of distillation column 2 and cucurbit 1, thus be conducive to steaming of the distillate in cucurbit 1, the efficiency according to device of the present invention can be improved on the one hand further, then can reduce the probability that cracking reaction at high temperature occurs distillate further on the other hand.Therefore, one of the present invention preferred embodiment in, the volume of described cucurbit 1 is 0.1-1 liter, and the length of described distillation column 2 (that is, distillates the column length between position from cucurbit top to distillate; Also namely, from the cucurbit position crossing with distillation column to the column length between the lower edge of the arm of distillation column) be 10-50mm.The length of described distillation column 2 is more preferably 30-45mm.
According to method of the present invention, as shown in Figure 1, described distillation column 2 preferably has insulation jacket 3, the outer wall of distillation column 2 and external environment are kept apart by described insulation jacket 3, the effect of insulation can be played, the phenomenon of further minimizing steam condensing backflow, and then the time of vacuum distillation can be shortened further.The various insulation jacket that can realize above-mentioned functions that described insulation jacket can be commonly used for this area, are not particularly limited.
According to the present invention, the distillation unit of described vacuum distillation plant preferably has the stirring apparatus for stirring the distillate in described cucurbit 1, and can make in still-process like this, distillate is heated evenly.According to the present invention, described stirring apparatus is preferably magnetic agitation, distillate can be made to be heated evenly so on the one hand, also can not have a negative impact to the impermeability of distillation unit on the other hand.
According to method of the present invention, described distillation unit can also comprise the temperature sensor for measuring steam temperature and distillate temperature.The present invention is not particularly limited for the kind of described temperature sensor and installation site, can be that the routine of this area is selected.Such as, can be lower to concordant by temperature sensor is inserted into the arm 5 of described distillation column 2 from the interface the vertical tube 4 of described distillation column 2, thus detect steam temperature.Again such as, when measuring the distillate temperature in cucurbit, by arranging interface on described cucurbit 1, temperature sensor can be inserted in distillate by this interface, thus detect distillate temperature.From the bubble-tight angle improving described vacuum distillation plant further, in the distillation unit of described vacuum distillation plant, preferred employing can detect the double temperature sensor of the temperature of two positions simultaneously, arm 5 times steam temperatures along place of the distillate temperature simultaneously in detection cucurbit 1 and distillation column 2.
According to the present invention, described distillation unit can also contain other parts normally used in still-process, such as: condenser, distillate receiver and well heater, repeat no more herein.
Fig. 3 shows a kind of embodiment of the distillation unit of the vacuum distillation plant used in method of the present invention.According to this embodiment, described distillation unit comprise cucurbit 1, distillation column 2, insulation jacket 3, be positioned at described cucurbit 1 stirring magneton 7, can Simultaneously test distillate temperature and steam temperature double temperature sensor 8, 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 used in method of the present invention.In this embodiment, temperature sensor interface is provided with above the side of cucurbit 1, temperature sensor 14 stretches in the distillate in cucurbit 1 by this interface, for detecting 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, pipeline between described vacuum unit and described distillation unit preferably arranges vacuum cold trap, with trapping from the condensability oil gas the air-flow that described distillation unit is extracted out, the pressure in vacuum distillation plant can be reduced on the one hand further, then can prevent on the other hand the oil gas coming from distillation unit from entering in the vacuum pump of 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 be that the routine of this area is selected.According to the present invention, described vacuum cold trap can make vacuum cold trap remain low temperature, to trap from the condensability oil gas in the air-flow of described distillation unit by using the method for cooling liquid.
The present invention is not particularly limited for the kind of described cooling liquid, can be conventional various cooling liquids, such as: liquid nitrogen.The present invention is also not particularly limited for the temperature of described liquid coolant, as long as the temperature of described liquid coolant is enough to guarantee condensability oil gas condensation.Preferably, the temperature of described liquid coolant is-120 DEG C to-60 DEG C.
The present invention is also not particularly limited for the structure of described vacuum cold trap, can be that the routine of this area is selected.Such as, the vacuum trap body of described vacuum cold trap can be U-shaped, the space that vacuum trap body surrounds may be used for holding liquid coolant, the gas access that the sidewall of described vacuum trap body is oppositely arranged and gas vent, wherein, described gas access is connected with described distillation unit, and described gas vent is connected with described vacuum unit.Again such as, the vacuum trap body of described vacuum cold trap can be cup type, and 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.
The present inventor is in research process, although arrange the amount that vacuum cold trap can reduce the condensable gas entering described vacuum unit between described vacuum unit and described distillation unit, but due to the low and synthermal height such as the normal pressure of the cut distillated of the pressure in the distillation unit of method according to the present invention, the content of the condensability oil gas in the air-flow thus pumped out from distillation 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 is found by great many of experiments, by arranging a mozzle in the vacuum trap body of described vacuum cold trap, the air-flow from described distillation unit is guided to enter in vacuum trap body along the inwall that described vacuum trap body contacts with liquid coolant, make air-flow can contact with the cooling wall of vacuum cold trap once entering vacuum trap body like this, thus improve the cooling effectiveness of vacuum cold trap further.
One of the present invention preferred embodiment in, as shown in Figure 5, described vacuum cold trap comprises the vacuum trap body 18 that cross section is U-shaped, 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, described gas access 19-1 is arranged on described mozzle 16 through the sidewall of vacuum trap body 18, described gas vent 19-2 is arranged on the sidewall of described vacuum trap body 18, air-flow is made to leave described vacuum trap body 18 along the outer wall of described mozzle 16.
Method according to the present invention is not particularly limited for the pipeline connecting described distillation unit and described vacuum unit, can be that this area routine is selected, repeat no more herein.
Fig. 6 shows a kind of arrangement of the vacuum distillation plant used in method of the present invention.As shown in Figure 6, vacuum unit adopts the oil-sealed rotary pump and ODP that are connected in series, and wherein oil-sealed rotary pump is as the forepump of described ODP, during work, first the temperature of vacuum cold trap is reduced to less than-70 DEG C; Then start oil-sealed rotary pump, open manual vacuum switch valve 20,21 and 22, make the pressure in the cavity of ODP and distillation unit be below 100Pa; Then close manual vacuum switch valve 21, and start ODP and automatically control vacuum solenoid 23, regulate the unlatching ratio of described automatic control vacuum solenoid 23 according to the pressure in predetermined distillation unit; When the pressure in vacuum distillation plant is in 0.1-10Pa, cucurbit is heated, and control the degree of heat of heating arrangement, make distillate in cucurbit with the ramp of 6-8 DEG C/min; After having distillate to distillate, the degree controlling heating makes distillate distillate with the speed of 5-10mL/min.
Method according to the present invention comprises to be sent in described cucurbit by fraction oil of petroleum, distills, and receive the cut with different recovered (distilled) temperatures with cut receiver respectively under the condition that described vacuum unit vacuumizes described distillation unit.Particularly, described fraction oil of petroleum is sent in described cucurbit, carry out the mode that vacuum distillation measures its boiling range to comprise: fraction oil of petroleum is put into cucurbit, open vacuum unit, pressure in distillation unit is made to reach 0.1-10Pa, heating cucurbit, collects the distillate of initial boiling point, each distillation yield cut and the end point of distillation.Described each distillation yield cut preferably includes the distillate that percent by volume is respectively 5%, 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90% and 95%.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 namely obtaining this fraction oil of petroleum such as normal pressure.Described steam temperature converts by the various methods that this area can be adopted to commonly use, and to become the normal pressure of this cut etc. synthermal, and the steam temperature observed in still-process becomes normal pressure etc. synthermal by distillation conversion pressure by table 1 by the present invention.In addition, for the steam temperature do not provided in table 1, normal pressure etc. can be become synthermal by the formula scales provided in the appendix A 7 of method of interpolation or ASTMD1160-06.It is the formula scales that provides in the appendix A 7 by ASTMD1160-06 in the embodiment of the present invention.
Table 1
According to method of the present invention, described fraction oil of petroleum can be the fraction oil of petroleum in various source.Preferably, described fraction oil of petroleum is by carrying out deep drawing wax oil that deep drawing obtains and/or deep drawing residual oil to long residuum or vacuum residuum.
When method of the present invention is carried out decompression distillation to fraction oil of petroleum (particularly deep drawing wax oil or deep drawing wax oil), the cut distillated can comprise the synthermal cut for 540-720 DEG C such as normal pressure.
The present invention is described in detail below in conjunction with embodiment.
Embodiment 1-10 is used for the method according to mensuration fraction oil of petroleum boiling range of the present invention is described.
Embodiment 1
Adopt the device shown in Fig. 6, wherein, distillation unit as shown in Figure 3, distillation column length is 35mm, distillation column as shown in Figure 2, anti-return pipe is inclined in the vertical tube of distillation column, and is benchmark with surface level, and 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 engages with the inwall place of the inwall of described arm at described vertical tube, and the bottom engaged with the inwall of described arm of described anti-return pipe is 0.5 to the minor increment of top end face of described anti-return pipe and the ratio of the internal diameter of described arm; Adopt the vacuum cold trap shown in Fig. 5.
91.85 grams of Chad No. 2 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 DEG C; Then start oil-sealed rotary pump, open manual vacuum switch valve 20,21 and 22, make the pressure in the cavity of ODP and distillation unit be 100Pa; Then close manual vacuum switch valve 21, and start ODP and automatically control vacuum solenoid 23; When to distill the pressure in unit be 0.1Pa, cucurbit heated, and controls the degree of heat of heating arrangement, make distillate in cucurbit with the ramp of 6 DEG C/min; After having distillate to distillate, the degree controlling heating makes distillate distillate with the speed of 5mL/min, records steam temperature when each cut distillates and pressure in still-process.
The steam temperature obtained is converted into normal pressure etc. by table 1 synthermal, obtain the boiling range data of Chad's No. 2 deep drawing wax oils, result illustrates in table 2.
Table 2
| Distillation yield (volume %) | Normal pressure etc. synthermal (DEG C) |
| 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 |
Embodiment 2
Adopt the device shown in Fig. 6, wherein, distillation unit as shown in Figure 3, distillation column length is 35mm, distillation column as shown in Figure 2, anti-return pipe is inclined in the vertical tube of distillation column, and is benchmark with surface level, and 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 engages with the inwall place of the inwall of described arm at described vertical tube, and the bottom engaged with the inwall of described arm of described anti-return pipe is 0.1 to the minor increment of top end face of described anti-return pipe and the ratio of the internal diameter of described arm; Adopt the vacuum cold trap shown in Fig. 5.
90.09 grams of Ackers are entangled the cucurbit that guest's deep drawing wax oil is placed in 500mL, then carries out vacuum distillation according to following flow process.
First the temperature of vacuum cold trap is reduced to-75 DEG C; Then start oil-sealed rotary pump, open manual vacuum switch valve 20,21 and 22, make the pressure in the cavity of ODP and distillation unit be 90Pa; Then close manual vacuum switch valve 21, and start ODP and automatically control vacuum solenoid 23; When to distill the pressure in unit be 1Pa, cucurbit heated, and controls the degree of heat of heating arrangement, make distillate in cucurbit with the ramp of 7 DEG C/min; After having distillate to distillate, the degree controlling heating makes distillate distillate with the speed of 8mL/min, records steam temperature when each cut distillates and pressure in still-process.
The steam temperature obtained is converted into normal pressure etc. by table 1 synthermal, obtain the boiling range data that Acker entangles guest's deep drawing wax oil, result illustrates in table 3.
Table 3
| Distillation yield (volume %) | Normal pressure etc. synthermal (DEG C) |
| 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 |
Embodiment 3
Adopt the device shown in Fig. 6, wherein, distillation unit as shown in Figure 3, distillation column length is 45mm, distillation column as shown in Figure 2, anti-return pipe is inclined in the vertical tube of distillation column, and is benchmark with surface level, and 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 engages with the inwall place of the inwall of described arm at described vertical tube, and the bottom engaged with the inwall of described arm of described anti-return pipe is 0.3 to the minor increment of top end face of described anti-return pipe and the ratio of the internal diameter of described arm; Adopt the vacuum cold trap shown in Fig. 5.
90.50 grams of instrument long lines deep drawing wax oils are placed in the cucurbit of 500mL, then carry out vacuum distillation according to following flow process.
First the temperature of vacuum cold trap is reduced to-90 DEG C; Then start oil-sealed rotary pump, open manual vacuum switch valve 20,21 and 22, make the pressure in the cavity of ODP and distillation unit be 80Pa; Then close manual vacuum switch valve 21, and start ODP and automatically control vacuum solenoid 23; When to distill the pressure in unit be 10Pa, cucurbit heated, and controls the degree of heat of heating arrangement, make distillate in cucurbit with the ramp of 8 DEG C/min; After having distillate to distillate, the degree controlling heating makes distillate distillate with the speed of 10mL/min, records steam temperature when each cut distillates and pressure in still-process.
The steam temperature obtained is converted into normal pressure etc. by table 1 synthermal, obtain the boiling range data of instrument long lines deep drawing wax oil, result illustrates in table 4.
Table 4
| Distillation yield (volume %) | Normal pressure etc. synthermal (DEG C) |
| 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 |
Embodiment 4
Adopt the method identical with embodiment 1 to carry out vacuum distillation to card human relations deep drawing wax oil, the boiling range data obtained illustrate in table 5.
Table 5
| Distillation yield (volume %) | Normal pressure etc. synthermal (DEG C) |
| 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 |
Embodiment 5
Adopt the method identical with embodiment 3 to carry out vacuum distillation to DOPA deep drawing wax oil, the boiling range data obtained are shown in table 6.
Table 6
| Distillation yield (volume %) | Normal pressure etc. synthermal (DEG C) |
| 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 |
Embodiment 6
Adopt the method identical with embodiment 1 to carry out vacuum distillation to Kuwait's deep drawing wax oil, the boiling range data obtained illustrate in table 7.
Table 7
| Distillation yield (volume %) | Normal pressure etc. synthermal (DEG C) |
| 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 obtained illustrate in table 8.
Table 8
| Distillation yield (volume %) | Normal pressure etc. synthermal (DEG C) |
| 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 obtained are shown in table 9.
Table 9
| Distillation yield (volume %) | Normal pressure etc. synthermal (DEG C) |
| 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 |
Embodiment 9
Adopt the method identical with embodiment 1 to Asia, Witter hereby deep drawing wax oil carry out vacuum distillation, the boiling range data obtained illustrate in table 10.
Table 10
| Distillation yield (volume %) | Normal pressure etc. synthermal (DEG C) |
| 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 |
Embodiment 10
Adopt the device shown in Fig. 6, wherein, distillation unit as shown in Figure 4, distillation column length is 35mm, distillation column as shown in Figure 2, anti-return pipe is inclined in the vertical tube of distillation column, and is benchmark with surface level, and 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 engages with the inwall place of the inwall of described arm at described vertical tube, and the bottom engaged with the inwall of described arm of described anti-return pipe is 0.3 to the minor increment of top end face of described anti-return pipe and the ratio of the internal diameter of described arm; Adopt the vacuum cold trap identical with the vacuum cold trap shown in Fig. 5, mozzle is not set unlike in the vacuum trap body of vacuum cold trap.
90.51 grams of 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 DEG C; Then start oil-sealed rotary pump, open manual vacuum switch valve 20,21 and 22, make the pressure in the cavity of ODP and distillation unit be 100Pa; Then close manual vacuum switch valve 21, and start ODP and automatically control vacuum solenoid 23; When to distill the pressure in unit be 10Pa, cucurbit heated, and controls the degree of heat of heating arrangement, make distillate in cucurbit with the ramp of 7 DEG C/min; After having distillate to distillate, the degree controlling heating makes distillate distillate with the speed of 5mL/min, records steam temperature when each cut distillates and pressure in still-process.
The steam temperature obtained is converted into normal pressure etc. by table 1 synthermal, obtain 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 (DEG C) |
| 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 display of embodiment 1-10, according to method of the present invention can synthermal to the normal pressure of cut etc. be that the fraction oil of petroleum of more than 590 DEG C carries out decompression distillation, and then obtain the boiling range data of this fraction oil of petroleum.
Claims (10)
1. one kind measures the method for 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 that there is the synthermal cuts such as different normal pressures, described vacuum distillation plant comprises vacuum unit and distillation unit, pipeline connection is passed through between described vacuum unit and distillation unit, described distillation unit comprises cucurbit and distillation column, the method comprises to be sent in described cucurbit by fraction oil of petroleum, 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, vacuum pump in described vacuum unit comprises the oil-sealed rotary pump and ODP that are connected in series, described oil-sealed rotary pump is as the forepump of described ODP,
The arm that described distillation column comprises vertical tube and stretches out from the side of described vertical tube, described arm is downward-sloping, described distillation column also comprises the anti-return pipe be arranged in described vertical tube, the bottom outer wall of described anti-return pipe connects with the inwall of described vertical tube, spacing is left between the top outer wall of described anti-return pipe and the inwall of described vertical tube, the bottom outer wall of described anti-return pipe engages with the inwall place of the inwall of described arm at described vertical tube, for being guided to by withdrawing fluid in described arm;
Pipeline between described distillation unit and described vacuum unit is provided with vacuum cold trap, described vacuum cold trap comprises the vacuum trap body that cross section is U-shaped, be nested in the mozzle in described vacuum trap body, the gas access be oppositely arranged and gas vent, the space that described vacuum trap body surrounds is for holding liquid coolant, 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, described gas access is arranged on described mozzle through the sidewall of described vacuum trap body, described gas vent is arranged on the sidewall of described vacuum trap body, air-flow is made to leave described vacuum trap body along the outer wall of described mozzle.
2. method according to claim 1, wherein, the volume of described cucurbit is 0.1-1 liter, and the length of described distillation column is 10-50mm.
3. method according to claim 1, wherein, described distillation column has insulation jacket.
4. method according to claim 1, wherein, described anti-return pipe is obliquely installed.
5. method according to claim 4, 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.
6. method according to claim 1, wherein, the bottom engaged with the inwall of described arm of described anti-return pipe is 0.1-0.5:1 to the minor increment of top end face of described anti-return pipe and the ratio of the internal diameter of described arm.
7. method according to claim 1, wherein, the cross section of described anti-return pipe is splayed.
8. method according to claim 1, wherein, use described vacuum distillation plant to carry out to fraction oil of petroleum the mode that vacuum distillation measures its boiling range to comprise: fraction oil of petroleum is put into cucurbit, open vacuum unit, pressure in distillation unit is made to reach 0.1-10Pa, heating cucurbit, collects the distillate of initial boiling point, each distillation yield cut and the end point of distillation.
9. the method according to claim 1 or 8, wherein, described cut comprises the synthermal cut for 540-720 DEG C such as normal pressure.
10. the method according to claim 1 or 8, 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 |
| CN105675645B (en) * | 2016-03-02 | 2019-03-05 | 南京理工大学 | Adiabatic calorimetry instrument anti-return component |
| 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 |
| 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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