Diesel oil solidifying point, cold filter clogging temperature line simultaneous analysis method and device thereof
Technical field
The invention belongs to oil quality on-line analysis field in the oil refining production run, relate in particular to a kind of diesel oil solidifying point, cold filter clogging temperature line simultaneous analysis method and device thereof.
Background technology
Diesel oil solidifying point, cold filter clogging temperature are two important quality index that indicate the diesel oil at low-temperature characteristic, in the oil refining production run, monitor these two indexs in real time, can the guiding operation workman in time revise operation, realization is controlled the diesel quality edge, improve diesel yield to greatest extent, economic benefit is very remarkable.Therefore reliable and stable diesel oil solidifying point, cold filter clogging temperature in-line analyzer just become the most important thing.
Current market leading products are the PSG44675 type cold filter clogging temperature analyser and the general pour point analyser of PSG44670 type of U.S. GCA company, and its basic structure is:
Referring to shown in Figure 1, it comprises test cabinet 101, sample measurement head 102, screen modules 103, temperature element 104, refrigeration module 105, cooling water tank 106, differential pressure transmitter 107;
Logical circuit 108, pressure pulse savings U type pipe 109, malleation conduit 110, negative pressure catheter 111;
Solenoid valve for sampling 112, stock layout solenoid valve 113, overflow solenoid valve 114, pressure pulse apply solenoid valve 115, pressure pulse savings solenoid valve 116, malleation emptying solenoid valve 117, negative pressure emptying solenoid valve 118.
Its principle of work is:
(1) oil-feed sample: solenoid valve 112,114 is opened all the other closed electromagnetic valves.
(2) oil sample cooling: all closed electromagnetic valves, refrigeration module 105 powers up.
(3) transmitter makes zero, the pressure pulse savings: emptying solenoid valve 117,118, pneumatic pressure pulses savings solenoid valve 116 are opened all the other closed electromagnetic valves.
(4) test solidifying point: pneumatic pressure pulses applies solenoid valve 115 and opens, the low-pressure air of savings in U type pipe is diffused into test cabinet, directly act on the plemum of differential pressure transmitter 107, and pass to the negative pressure chamber of differential pressure transmitter 117 through oil sample, screen modules 103, sample measurement head 102, equal to apply pressure pulse one time.
Whenever apply pressure pulse one time, detect transmitter output signal and set-point relatively,, repeat (3), (4) operation if be lower than set-point.Illustrate constantly that until transmitter output signal 〉=set-point filter screen stops up, the output valve of this moment temperature element 104 is exactly the oil sample cold filter clogging temperature.
It is same that the general pour point of PSG-44670 type (solidifying point) instrument that the said firm produces and a PSG-44675 type filter point instrument have only, and cancelled screen modules 103, and set-point changes that little all the other are just the same, repeats no more.
The feature of prior art and the deficiency of existence:
(1) makes the test cabinet cooling according to semiconductor cooler.(2) make the oil sample in the test cabinet produce fine motion according to applying the external pressure pulse.(3) periodically detect oil sample dynamic viscous resistance drop and set-point comparison with differential pressure transmitter.(4) analytical cycles are made up of a plurality of sense cycle.(5) each sense cycle, differential pressure transmitter will be returned once zero; Pneumatic pressure pulses of U type Guan Yaochong storage is pressed in storage; Solenoid valve wants repetitive operation once.(6) analysis precision was associated with the duplicate detection cycle, and the big precision of long detection aperture of cycle is just poor; The little precision height of short detection aperture of repetition period, but solenoid valve frequent movement, the life-span will shorten greatly.
Owing to the method for above-mentioned detection oil sample dynamic viscous resistance, determined the complicacy of its structure; Also determined to detect periodicity relatively and two kinds of apparatus structure height repetitions, cost is improved greatly.Owing to detect periodicity relatively, determined the long and low situation of analysis precision of analytical cycle.PSG-44675 cold filter clogging temperature analyser, repeatable accuracy nominal value: ± 1 ℃.PSG-44670 pour point (solidifying point) analyser, repeatable accuracy nominal value: ± 2.5 ℃.
Summary of the invention
Problem to be solved by this invention is to have overcome the deficiencies in the prior art, a kind of diesel oil solidifying point, cold filter clogging temperature line simultaneous analysis method and device thereof are provided, it integrates solidifying point, cold filter clogging temperature is analyzed, need not to apply the external pressure pulse, oil sample static pressure in same analytical cycle in the watch-keeping temperature-fall period changes, and reaches threshold value and gathers solidifying point and cold filter clogging temperature value at once.
Technical matters to be solved by this invention takes following scheme to realize:
1. the method for a diesel oil solidifying point, cold filter clogging temperature line simultaneous analysis, it is realized with following step:
The oil sample displacement
First oil sample displacement solenoid valve, oil sample are replaced total solenoid valve and are opened, all the other closed electromagnetic valves, and with the old oil sample in new oil sample displacement cold filter clogging temperature analysis oil extraction pipeline and the analysis chamber, old oil sample flows into the oil sample recover through the overflow vent petroleum pipeline;
Second oil sample displacement solenoid valve, oil sample are replaced total solenoid valve and are opened, all the other closed electromagnetic valves, and with the old oil sample in new oil sample displacement pilot pipeline and the analysis chamber, old oil sample flows into the oil sample recover through the overflow vent petroleum pipeline;
The refrigeration cooling
Power up for two semiconductor coolers, the emptying solenoid valve is opened, and all the other closed electromagnetic valves allow the analysis chamber lower the temperature gradually;
The monitoring solidifying point
The output of computing machine continuous detecting differential pressure transmitter is carried out computing and threshold ratio, in the moment more than or equal to threshold value, gathers temperature element output, shows after the computing and solidifies point value;
Stop cold recovery
Give two semiconductor cooler outages, first oil sample displacement solenoid valve, emptying solenoid valve are opened, and all the other closed electromagnetic valves heat up the analysis chamber gradually;
The monitoring cold filter clogging temperature
By computing machine continuous detecting differential pressure transmitter output valve, go forward side by side row operation and threshold ratio, constantly, gather the output valve of temperature element more than or equal to threshold value, show the cold filter clogging temperature value after the computing, finish an analytical cycle.
Technical matters to be solved by this invention can also take following scheme to realize:
Method as the aforementioned, the basis for estimation of described solidifying point, cold filter clogging temperature is to be drawn by following analysis mode:
P
3=P
2/P
1
=H
Y·M
Y·P(T
2)/H
Y·M
Y
=P(T
2)…………(4)
Wherein: P
1=H
YM
Y
P
1Be the force value of test tube oil sample before by refrigeration;
P
2=H
Y·M
Y·P(T
2)
P
2Be that the test tube oil sample is arrived solidifying point force value constantly by refrigeration;
P (T
2) be the decompression coefficient;
H
Y: test tube liquid is annotated height;
M
Y: test tube liquid is annotated density;
T
2: the test tube oil sample is by the time of refrigeration to solidifying point.
2. according to a kind of diesel oil solidifying point of using in the aforesaid method, cold filter clogging temperature line simultaneous analysis device,
This device is the center to analyze chamber, descends two ends respectively through upper and lower heat-insulated pipe, fixedly connected in the static pressure mode with upper and lower oil circuit board thereon; On two sides, the described analysis chamber left and right sides first refrigerator, second refrigerator are installed respectively, in described analysis chamber front or back first connecting pipe be communicated with following oil circuit board; Net-filter assembly is installed in the indoor below of analysis cavity;
In first refrigerator outside first cooling water tank 308 is installed, second cooling water tank is installed in second refrigerator outside;
Last oil circuit plate top surface is installed a temperature element, and the temperature element lower end reaches and analyze the chamber middle part, and last oil circuit board side oil sample overflow vent is communicated with the oil sample recover through petroleum pipeline;
Following oil circuit board left side or right side oil sample displacement mouth are communicated with once first petroleum pipeline and first oil sample displacement electromagnetic valve outlet;
Following oil circuit board left side or right side oil sample displacement mouth two are communicated with through second petroleum pipeline and second oil sample displacement electromagnetic valve outlet;
A following oil circuit board left side or right side static pressure sample tap are communicated with the differential pressure transmitter plemum through connecting pipe, and differential pressure transmitter negative pressure chamber is communicated with atmosphere;
The inlet of first oil sample displacement solenoid valve is replaced total electromagnetic valve outlet with the inlet of second oil sample displacement solenoid valve with oil sample and is communicated with through petroleum pipeline with the emptying electromagnetic valve entrance, oil sample is replaced total electromagnetic valve entrance and is communicated with the oil sample acquisition port, and the emptying electromagnetic valve outlet is communicated with the oil sample recover;
The electric signal end of differential pressure transmitter, temperature element and all solenoid valves is connected with computing machine respectively.
Above-mentioned method, principle is definite, and its apparatus structure is simple, can make the cost of instrument reduce by one times; Can make user's water, electricity, gas, oil consumption save one times; Work efficiency doubles.The replicate analysis precision reaches ± and 0.5 ℃, be better than PSG-44670 and PSG-44675.Be better than national standard " GB510, GB386 ".
Description of drawings:
Fig. 1 is the structural representation of located by prior art;
Fig. 2 is a test unit synoptic diagram of the present invention;
Fig. 3 is the structural drawing of apparatus of the present invention;
Fig. 4 is that the C-C of Fig. 3 is to cut-open view.
Specific embodiment
Referring to Fig. 2, mechanism of the present invention is described by experiment.
We can get one 300 millimeters high test tubes (201), open a hole in its bottom, are connected with an atmospheric valve (203) through mozzle (202).The filter screen (204) of a slice 363 molybdenums is in vitro installed at 34 millimeters places in the distance bottom; Locate to open on the test tube wall hole for 50 millimeters in the distance bottom again, be connected with differential pressure transmitter (206) plemum through connecting pipe (205), differential pressure transmitter negative pressure chamber communicates with atmosphere.The signal output part of differential pressure transmitter connects a pressure digital display meter (207).A temperature element (208) in vitro is installed again, and the temperature element output terminal connects a deblocking temperature digital display meter (209).The diesel oil standard sample of specified temp is slowly poured into test tube, make the pressure digital display meter show a steady state value.Preliminary work is ready, and test tube is put into cold-trap (210) pull-down test.
The zero hour, temperature reduced gradually, and static pressure is constant; Static pressure also began slowly to reduce with the reduction of temperature and is more and more faster afterwards, noted noting the static pressure of solidifying point correspondence.So far finish the preceding semiperiod of a test period.
Take out test tube and open test tube bottom atmospheric valve, the recuperation of observing oil sample temperature and static pressure at normal temperatures, because inertia, the zero hour, temperature and static pressure continued all to descend that just speed is more and more slower in zero; Then temperature and all bottom outs of static pressure, speed are equally more and more slower in zero; Then temperature continues the rise static pressure and begins decline, at this moment will note writing down the static pressure of cold filter clogging temperature correspondence, and so far a test period finishes.
Such test can repeat tens times even hundreds of time, and examination keeps a record, and we can find that with the corresponding gang's static pressure of solidifying point almost be identical; Gang's static pressure of cold filter clogging temperature correspondence almost also is identical.Solidifying point static pressure and cold filter clogging temperature static pressure are asked the analysis criterion that has on average just obtained solidifying point and cold filter clogging temperature respectively, the criterion that but obtains so only is applicable to the condition of specific oil sample temperature, on-line analysis in the actual production process, the oil sample temperature fluctuates within the specific limits.
As follows according to aforesaid analysis of experiments mechanism:
Solidifying point is analyzed
Because the viscosity resistance F of oil product
NThe function that is temperature T is F
N=F (T); The volume V of oil product
YThe function that also is temperature T is V
Y=V (T).The density M of oil product
YThe double base function that is temperature T and component branch rate I is M
Y=M (T, I).
It highly is constant that diesel oil liquid so we must guarantee to pack at every turn in the test tube is annotated; The oil sample temperature is constant, thereby guarantees that the detected initial static pressure P of differential pressure transmitter is constant.
P=H
Y·M
Y。…………(1)
H
Y: test tube liquid is annotated height.M
Y: test tube liquid is annotated density.
When test tube was lowered the temperature gradually by refrigeration, the viscosity resistance of oil sample reduced with temperature that to rise be T ↓ F in the test tube
N↑; It is T ↓ V that the volume of oil sample dwindles with the temperature reduction
Y↓.Because these two kinds of phenomenon generation speed are different, F
N↑ change fast; V
Y↓ change slowly, therefore caused the generation of slight void in the test tube, we call liquid to this phenomenon and annotate by the phenomenon of soaring in the temperature-fall period.
Before making the test tube oil sample by refrigeration, the detected static pressure of differential pressure transmitter is P
1=P; The test tube oil sample is arrived solidifying point T by refrigeration
2Constantly, the detected static pressure of differential pressure transmitter is P
2, the above-mentioned just phenomenon of soaring makes P
2<P
1, therefore obtain:
P
1=H
Y·M
Y…………(2)
P
2=H
Y·M
Y·P(T
2)…………(3)
P (T in the formula
2) being the decompression coefficient, we call the effect of soaring to this decompression phenomenon.
Oil sample temperature, component divide rate all to change within the specific limits in the actual production process, so M in the following formula
Y(T I) is the uncertain factor to=M, and (3) formula can not be directly as the solidifying point criterion.
Make P
3=P
2/ P
1
=H
Y·M
Y·P(T
2)/H
Y·M
Y
=P(T
2)…………(4)
By the visible static pressure P of (4) formula
3With solidifying point T
2Unique correspondence, P
3As the solidifying point criterion, the replicate analysis precision can reach ± and 0.5 ℃, be better than national standard " GB510 ".
Cold filter clogging temperature is analyzed
National standard (GB386) specified test is: cooling samples and at 1961Pa (200mmH under defined terms
2O) pressure suction down makes sample pass through one 363 molybdenum filtrator.When sample is cooled to uniform temperature,, measure blocking filter temperature constantly with 1 ℃ of cooling at interval.
The suction method of being said among the GB386 is to keep filter screen simultaneously to be atmospheric pressure state, and another side is negative pressure 200mmH
2The O state, the differential pressure value on filter screen two sides is 200mmH like this
2O.Static pressure analytical approach of the present invention is that maintenance filter screen bottom surface is an atmospheric pressure state, utilizes oil sample liquid to annotate above and highly produces malleation 200mmH
2The O state, the differential pressure value on same filter screen two sides is 200mmH
2O.
The suction method of being said among the GB386 is to seek filter screen just to have stopped up temperature constantly in the oil sample temperature-fall period.Static pressure method that this paper says is the process of the low-temperature condition temperature recovery of oil sample below solidifying point, seeks filter screen and has just dredged temperature constantly.Above-mentioned solidifying point is analyzed criterion formula (4) and is equally applicable to filter point analysis, no longer repeats.According to this cold filter clogging temperature replicate analysis precision can reach ± 0.5 ℃.Be better than national standard " GB386 "
See also Fig. 3, Fig. 4, the analysis chamber made from fine copper or pure aluminum material (301) is the center, descends two ends to be connected with upper and lower oil circuit board (304), (305) static pressure of aluminium alloy or copper alloy made through upper and lower heat-insulated pipe (302), (303) that polytetrafluoroethylmaterial material is made respectively thereon; Be connected with cooling water tank (308), (309) static pressure through first semiconductor cooler (306), second semiconductor cooler (307) respectively on its two sides, left and right sides; First connecting pipe (310) that (back) face is made through thermal insulation material before it is communicated with following oil circuit board; Net-filter assembly (311) is installed in the indoor below of analysis cavity.
Last oil circuit plate top surface is installed by a temperature element (312) and the temperature element lower end reaches analysis chamber middle part.Last oil circuit board side oil sample overflow vent is communicated with the oil sample recover through petroleum pipeline (313).
An one of following oil circuit board left side (right side) side oil sample displacement mouth is communicated with through petroleum pipeline (314) and first oil sample displacement solenoid valve (315) outlet.Two of a following oil circuit board left side (right side) side oil sample displacement mouth is replaced solenoid valve (317) outlet through the petroleum pipeline (316) and second oil sample and is communicated with.A following oil circuit board left side (right side) side static pressure sample tap is communicated with differential pressure transmitter (319) plemum through second connecting pipe (318), and differential pressure transmitter negative pressure chamber is communicated with atmosphere.
First oil sample displacement solenoid valve (315) inlet is replaced total solenoid valve (320) outlet with second oil sample displacement solenoid valve (317) inlet and oil sample and is communicated with through petroleum pipeline with emptying solenoid valve (321) inlet.Oil sample is replaced total solenoid valve (320) inlet and is communicated with the oil sample acquisition port, and emptying solenoid valve (321) outlet is communicated with oil sample recover (322).
The electric signal end of differential pressure transmitter (319), temperature element (312), all solenoid valves (315), (317), (320), (321) is connected with computing machine respectively, for computing machine provides acquired signal and is controlled by computing machine (323).
The above, it only is preferred embodiment of the present invention, be not that the present invention is done any type of restriction, every foundation technical spirit of the present invention is done any simple modification, equivalent variations and modification to above embodiment, all belongs to the scope of technical solution of the present invention.