CN103254937B - Hydrocarbon oil dewaxing experimental instrument and experimental method thereof - Google Patents
Hydrocarbon oil dewaxing experimental instrument and experimental method thereof Download PDFInfo
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- CN103254937B CN103254937B CN201310159286.3A CN201310159286A CN103254937B CN 103254937 B CN103254937 B CN 103254937B CN 201310159286 A CN201310159286 A CN 201310159286A CN 103254937 B CN103254937 B CN 103254937B
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- 238000002474 experimental method Methods 0.000 title claims abstract description 63
- 239000004215 Carbon black (E152) Substances 0.000 title claims abstract description 31
- 229930195733 hydrocarbon Natural products 0.000 title claims abstract description 31
- 150000002430 hydrocarbons Chemical class 0.000 title claims abstract description 31
- 239000002904 solvent Substances 0.000 claims abstract description 230
- 238000000034 method Methods 0.000 claims abstract description 39
- 238000012360 testing method Methods 0.000 claims description 109
- 238000003756 stirring Methods 0.000 claims description 24
- 238000000967 suction filtration Methods 0.000 claims description 24
- 238000001914 filtration Methods 0.000 claims description 17
- 238000005057 refrigeration Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 11
- 239000012065 filter cake Substances 0.000 claims description 10
- 238000005086 pumping Methods 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000013459 approach Methods 0.000 claims description 6
- 239000013557 residual solvent Substances 0.000 claims description 6
- 238000001073 sample cooling Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000013461 design Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 2
- 231100000481 chemical toxicant Toxicity 0.000 abstract 1
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 239000003440 toxic substance Substances 0.000 abstract 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 54
- 239000001993 wax Substances 0.000 description 26
- 239000000047 product Substances 0.000 description 18
- 239000000203 mixture Substances 0.000 description 9
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- 230000009897 systematic effect Effects 0.000 description 5
- 238000009434 installation Methods 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 239000003507 refrigerant Substances 0.000 description 2
- 208000028571 Occupational disease Diseases 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004807 desolvation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000009916 joint effect Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000002277 temperature effect Effects 0.000 description 1
Abstract
The invention discloses a hydrocarbon oil dewaxing experimental instrument and an experimental method thereof. According to the invention, a solvent cylinder and a filter cylinder which are the same as a sample cylinder in specification and dimension and have interchangeability are additionally arranged on the basis of the traditional hydrocarbon oil dewaxing experimental instrument, and the solvent cylinder, the filter cylinder and the sample cylinder are simultaneously positioned in a same cold bath, so that the consistency of solvent temperature, filter temperature and sample temperature is ensured in an experimental process, the difficulty of experimental operation and temperature control which needs to be respectively carried out on the sample cylinder, the solvent cylinder and the filter cylinder in the experimental process, the system errors of an experimental result are decreased, and the parallelism of the experimental result is enhanced; and the automation of solvent addition is realized by adding a solvent metering addition system, so that the labor intensity of manual operation in the experimental process is reduced, the contact opportunity of an experimental operator and toxic chemical components contained in the experimental solvent is reduced, and the occupational health of the experimental operator is favorable.
Description
Technical field
The present invention relates to a kind of laboratory apparatus and experimental technique thereof, relate in particular to a kind of hydrocarbon ils dewaxing laboratory apparatus and experimental technique thereof.
Background technology
The method of hydrocarbon ils dewaxing has a variety of, and wherein the most frequently used is solvent dewaxing process.The principle of solvent dewaxing mixes stock oil with dewaxing solvent exactly mutually, then cooling in control situation, utilize insoluble to wax the component at low temperatures or oligodynamical of solvent and characteristic to other components dissolved beyond paraffin removal, make wax crystallization in solution, solution is filtered, obtain dewaxed filtrate and slack wax, more separately respectively after desolvation, obtain pressed oil, gatch.
In prior art, the solvent dewaxing laboratory apparatus that hydrocarbon ils dewaxing experiment adopts is carried out in laboratory, generally only has a test specimen tube, each application of sample, all needing to use graduated cylinder to measure a certain amount of solvent adds in test specimen tube, sample need to be poured the sample in test specimen tube into cartridge filter and carry out suction filtration after stirring, dissolving.Due to, the mode that adds of solvent relies on manually and adds from outside, test specimen tube belongs to different equipment or device from cartridge filter, hydrocarbon ils dewaxing experimentation is for solvent, the temperature controlled levels of precision of sample and filtration procedure can only rely on operator's consummate experience and operating skill, owing to having the temperature difference between the initial temperature of solvent and specimen temperature, conventionally need to carry out the cooling of long period to solvent, until solvent temperature, be reduced to when consistent with specimen temperature and solvent could be joined in sample, after sample dissolution finishes, for keeping as far as possible homo(io)thermism in filtration procedure, be also one of key factor of experimental result accuracy.Therefore, in experimentation, conventionally need to expend the longer time, and experiment operator in experimentation, need constantly to the temperature of solvent monitor, control, skilled operation fast.And, in the last filtration procedure of sample, because envrionment temperature inevitably affects, between the temperature of strainer and specimen temperature, there is the temperature difference, will there is fluctuation in the temperature of whole filtration procedure, cause the systematic error of experimental result large.Once there is people therefore to expect solvent and strainer to be placed in refrigerator, wish to reduce solvent as far as possible, the temperature difference of strainer and sample, but owing to failing all the time to solve the interference of environmental factors in the solvent adition process of sample and filtration procedure, can not solve and rely on operator's operating skill and experience to sample, solvent, synchronism and the consistence of strainer temperature-fall period are controlled, whole experimentation is very large to the consumption of operator's energy, experimentation often need to consume the longer time, the systematic error of experimental result is larger, the collimation of experimental data also often cannot guarantee.
The present invention is by improving solvent dewaxing laboratory apparatus of the prior art, by test specimen tube, solvent drum and cartridge filter being integrated in same equipment, set up automatic control solvent and add the technique means such as system, the consistence that has kept solvent, strainer and specimen temperature to control, significantly reduce systematic error and the random error of experimental result, guaranteed accuracy and the collimation of experimental data.
On the other hand, due to dewaxing solvent, generally adopt the organic solvents such as toluene, two butanone, in experimentation, particularly solvent adds with filtration procedure and need to repeatedly be exposed in environment, the obnoxious flavour volatilizing in solvent can be avoided being sucked by experimenter, the healthy disadvantageous effect that causes to experimenter.The present invention adds system by increasing solvent, make except first solvent adds, other adition process is all undertaken by installing automatically under airtight state, and the filtration procedure of sample dissolution after finishing is also to carry out under airtight state, effectively reduce the volatilization of hazardous solvent composition in experiment place, be conducive to guarantee the Occupational health of experiment operator.
Summary of the invention
For solving above-mentioned problems of the prior art, the present invention proposes a kind of hydrocarbon ils dewaxing laboratory apparatus and experimental technique thereof, this experimentation Experiments of Automatic Control condition and avoid manual intervention, guarantees the accuracy of experiment and avoids the infringement of experiment to people.
For realizing the object of foregoing invention, the present invention is to having made corresponding technological improvement on existing use for laboratory hydrocarbon ils dewaxing laboratory apparatus basis, hydrocarbon ils dewaxing laboratory apparatus after improvement comprises main body frame, controller with digital display screen is installed in main body frame, liftable agitator, miniature volume pump, cryostat, test specimen tube, and pumped vacuum systems and refrigeration system outside device, wherein, pumped vacuum systems is connected with strainer, cryostat access refrigeration system refrigeration, liftable agitator be arranged on test specimen tube directly over, above-mentioned experiment solvent dewaxing device also includes solvent injected system, solvent drum, cartridge filter, described solvent injected system is by the miniature volume pump being controlled by the controller, T-valve and pipeline form, described miniature metering pump intake piping road is connected with described solvent drum, described T-valve is arranged on described miniature metering pump discharge pipe road, two exit end of described T-valve are connected with solvent drum with described test specimen tube respectively by pipeline, described strainer is connected with described pumped vacuum systems, described test specimen tube and described test specimen tube, when solvent drum and cartridge filter work, be placed in cryostat simultaneously, described test specimen tube, solvent drum is separately installed with cartridge filter the temperature sensor being connected with digital display screen.
Solvent dewaxing unit of the present invention is by setting up solvent drum and cartridge filter, and solvent drum, cartridge filter and test specimen tube are placed in to cryostat simultaneously, make solvent drum, test specimen tube and cartridge filter three temperature possess consistence, and control process is easier; Solved the solvent drum, the test specimen tube that in prior art, exist and laid respectively at different positions from cartridge filter, between each, needed respectively temperature-fall period and outlet temperature to be controlled, thus the experimental error of bringing manual intervention to produce.
Dewaxing device of the present invention is by setting up the miniature volume pump being controlled by the controller, the solvent injected system that T-valve and pipeline form, the above-mentioned miniature metering pump intake piping road being controlled by the controller is connected with described solvent drum, wherein T-valve is arranged on the miniature metering pump discharge pipe road being controlled by the controller, two exit end of T-valve are connected with solvent drum with described test specimen tube respectively by pipeline, cartridge filter and the technical measures such as described pumped vacuum systems is connected, make in experimentation, the solvent adition process of test specimen tube can be carried out automatically, in whole experimentation, remain that solvent drum and test specimen tube are placed in same cryostat simultaneously.Abovementioned technology has solved in prior art, fashionable owing to adding at test specimen tube solvent, need to solvent could be added to test specimen tube by the artificial repeated multiple times solvent drum that picks and places, thereby causes the problem of envrionment temperature on solvent drum and solvent temperature impact.
As mentioned above, set up after solvent injected system, from solvent drum, solvent is joined test specimen tube process implementation automatic control.Because test specimen tube, solvent drum and cartridge filter are separately installed with the temperature sensor being connected with digital display screen, in experimentation, experiment operator, by observing the temperature data on digital display screen, just can be determined adding opportunity of solvent according to the required temperature of each step of experiment easily;
What the introducing of T-valve had guaranteed that above-mentioned solvent adds carries out automatically, and make operator to the grasp of solvent adding amount and control easier with respect to prior art: when needs are when adding solvent in test specimen tube, the outlet gear of T-valve being adjusted to test specimen tube direction; When solvent adding amount reaches experiment demand in test specimen tube, the outlet gear of T-valve is adjusted to solvent drum direction.
In sum, the present invention, by setting up solvent drum and cartridge filter, is arranged on itself and test specimen tube on same hydrocarbon ils dewaxing laboratory apparatus, and solvent drum, cartridge filter and test specimen tube is placed in to same cryostat.Can guarantee like this solvent temperature and filter temperature and specimen temperature consistence, effectively reduce in experimental implementation and experimentation and need respectively test specimen tube, solvent drum and cartridge filter to be carried out to temperature controlled difficulty, reduced experimental result systematic error, improved the collimation of experimental result; Simultaneously, also reduced the temperature that operator in experimentation should control and observe solvent drum internal solvent, again must be according to sample in test specimen tube to solvent adding amount with add opportunity demand that the solvent in solvent drum is joined to the technical difficulty in test specimen tube, saved the time of experiment and the labour intensity of experimental implementation.
The miniature volume pump that the present invention is controlled by the controller by employing, and set up a T-valve on miniature metering pump outlet pipeline, two exit end of T-valve are accessed respectively to test specimen tube and solvent drum, test specimen tube, solvent drum and cartridge filter are separately installed with the temperature sensor being connected with digital display screen, and operator are by observing the flow direction of the data exchange T-valve outlet solvent showing on digital display screen.Like this, just can pass through by controller, the common solvent forming of miniature volume pump and T-valve adds system, by switching the flow direction of solvent, realized the automatic control that test specimen tube solvent adds, and due to test specimen tube, on solvent drum and cartridge filter, is all furnished with the tight upper cover of sealing, in the solvent automatization adition process of whole experiment, the chance of the direct solvent contact of operator significantly reduces, significantly reduced in prior art and frequently carried out the manual health harm that adds brought frequent direct solvent contact to cause of solvent because operator need experimental process, be conducive to reduce the occurrence risk of occupational illness.
As a kind of optimal technical scheme, hydrocarbon ils of the present invention dewaxing laboratory apparatus, its solvent drum, cartridge filter are consistent with the scantlings of the structure of described test specimen tube, possess interchangeability.The employing of technique scheme, is conducive to reduce maintenance and repair cost, reduces device fabrication cost; And after hydrocarbon ils dewaxing off-test, the cleaning of test specimen tube generally all needs the time of growing, test specimen tube, solvent drum and cartridge filter possess interchangeability to carry out continuously various sample and tests required sample setup time significantly accelerating laboratory.
As another kind of optimal technical scheme, the volume of the group/external member of the solvent drum of hydrocarbon ils laboratory apparatus of the present invention, cartridge filter and test specimen tube be one group/cover or many groups/cover, volume between each group/external member is different.
Adopt technique scheme, make hydrocarbon ils laboratory apparatus of the present invention can meet the needs of petrochemical industry laboratory to the experiment of multiple different material, different experimental program and different requirement of experiment etc.
According to the rule of thumb data in petrochemical industry laboratory, consider various various sample and various specific experiment requirement, three of optimal way, is that group/kit size specifications design of not isometric solvent drum, cartridge filter, test specimen tube is become to 0.5～5 liter.
The invention also discloses a kind of experimental technique that adopts hydrocarbon ils dewaxing laboratory apparatus of the present invention, comprise the following steps:
Preparation solvent preheating in water-bath; Take sample, join in solvent dewaxing equipment test specimen tube, in water-bath, heat, add the solvent of preheating and stir sample is dissolved completely;
Test specimen tube is taken out from water-bath, dry water, be placed in solvent dewaxing equipment; Open solvent dewaxing equipment, cryostat temperature is set, start refrigeration;
Residual solvent is added respectively to solvent drum and cartridge filter, strainer is put into cartridge filter, build each cover plate;
When specimen temperature drops to room temperature, start to add solvent; In adition process, constantly stir sample, observe sample cooling temperature, intermittent stirring sample;
When sample, solvent, filter temperature are all reduced to design temperature, from test specimen tube, take out agitator, the sample on agitator is recovered to test specimen tube;
From cartridge filter, take out strainer, put into the sample of test specimen tube, open pumping and filtering device, carry out suction filtration;
When sample liquid level approaches strainer, then add solvent, continue suction filtration;
Reclaim the solvent in filtrate and filter cake, obtain slack wax and pressed oil.
Experimental technique of the present invention, in the hydrocarbon ils dewaxing experimentation that its technical problem that will solve is prior art, relying on experiment operator self and remove to grasp and control experiment condition, there is many systematic errors and random error in the experimental technique that inevitably exists the externalitiess such as too much manual intervention and ambient temperature effect to cause.That is, there is the poor deficiency of experimental result accuracy and collimation.
The present invention adopts technique scheme, make experimentation Experiments of Automatic Control condition, effectively avoided manual intervention, both guaranteed accuracy and the collimation of experimental result, significantly reduced again in experimentation because solvent evaporates, be conducive to operator's Occupational health.
Accompanying drawing explanation
Fig. 1 is the two dimensional structure schematic diagram of hydrocarbon ils dewaxing laboratory apparatus;
Fig. 2 is the top plan view organigram of hydrocarbon ils dewaxing laboratory apparatus;
Fig. 3 is the perspective view of hydrocarbon ils dewaxing laboratory apparatus test specimen tube;
Fig. 4 is test specimen tube structural upright schematic diagram.
Embodiment
Fig. 1 is experiment solvent dewaxing apparatus structure schematic diagram.
Shown in Fig. 1 is a preferred embodiment of the present invention, experiment solvent dewaxing device shown in Fig. 1, comprise main body frame 1, controller 2, liftable agitator 3, cryostat 10, test specimen tube 4 with digital display screen are installed in main body frame, and above-mentioned use for laboratory hydrocarbon ils dewaxing laboratory apparatus is connected with refrigeration system 7 with the pumped vacuum systems 11 outside device.Wherein, pumped vacuum systems 11 is connected with cartridge filter 6, and cryostat 10 is connected with refrigeration system 7, and liftable agitator 3 is arranged on the top of test specimen tube 4.During work, agitator 3 moves down, and stirring-head falls in test specimen tube 4; After stirring completes, test specimen tube 4 is left in stirring-head lifting; In the present invention, the solvent drum 5 of setting up, cartridge filter 6, be arranged in same use for laboratory hydrocarbon ils dewaxing laboratory apparatus with test specimen tube 4, and the corresponding solvent injected system that has additional; The miniature volume pump 13 that employing is controlled by the controller, the inlet ductwork of miniature volume pump 13 is connected with solvent drum 5, a T-valve 12 is installed on the export pipeline of miniature volume pump 13, the entrance of this T-valve is connected with the exit end of miniature volume pump 13, and two other exit end of T-valve 12 is connected with solvent drum 5 with test specimen tube 4 respectively with the second pipeline 15 by the first pipeline 14; In figure, the 3rd pipeline 8 is respectively with the 4th pipeline 9 refrigerant feed conduit and the refrigerant return pipe road that the refrigeration system 7 outside device is connected with cryostat 10, above-mentioned cartridge filter 6 is connected (in figure, having omitted connecting pipeline) with the pumped vacuum systems 11 outside device, and said sample cylinder 4 is placed in cryostat 10 with solvent drum 5, cartridge filter 6 simultaneously while working.
Fig. 2 is the top plan view organigram of hydrocarbon ils dewaxing laboratory apparatus, and as can be seen from Figure 2 solvent drum 5, cartridge filter 6 are set up in parallel in hydrocarbon ils dewaxing laboratory apparatus with test specimen tube 4.
Fig. 3 is the perspective view of hydrocarbon ils dewaxing laboratory apparatus test specimen tube, can find out that test specimen tube 4, solvent drum 5 and cartridge filter 6 are placed on the situation in same cryostat 10 in figure.
Fig. 4 is the perspective view of hydrocarbon ils dewaxing laboratory apparatus test specimen tube, and solvent drum 5 is identical with internal structure and test specimen tube 4 with cartridge filter 6 contour structure sizes, so, omit and do not draw.Pilot hole 16 in figure on test specimen tube can be positioned on board panel by steady brace test specimen tube, avoids in agitator whipping process because stressed and cause test specimen tube to wave; On the solvent drum not drawing in figure, cartridge filter, also there is pilot hole, act on identical with the pilot hole on test specimen tube.
Adopt above-mentioned hydrocarbon ils dewaxing laboratory apparatus to carry out following two groups of contrast experiments:
First group of contrast experiment:
Experiment oil product: deasphalted oil;
Solvent: toluene and 2-butanone mixture, volume ratio is 1:1; Agent-oil ratio: about 6:1;
Experimental installation: solvent dewaxing equipment of the present invention
Experimentation: first configure solvent, add respectively 750ml toluene and 750ml2-butanone in 2L graduated cylinder, fully stir, mix standby;
The solvent that measures 400ml is preheating to 40 ℃ in water-bath;
Take sample oil product 200.0g, join in solvent dewaxing equipment test specimen tube, in water-bath, be heated to 40 ℃, add the solvent 400ml that is preheating to 40 ℃, stir sample is dissolved completely;
Open solvent dewaxing equipment, cryostat temperature is set and is-25 ℃, start refrigeration;
Test specimen tube is taken out from water-bath, dry water, be placed in solvent dewaxing equipment;
Residual solvent is added respectively to solvent drum and cartridge filter, and solvent drum adds solvent 900ml, and cartridge filter adds solvent 200ml, and strainer is put into cartridge filter, builds each cover plate;
When specimen temperature drops to room temperature, start to add solvent.Add 200ml at every turn, add altogether 3 times.In adition process, constantly stir sample, observe sample cooling temperature, intermittent stirring sample.When sample, solvent, filter temperature are all reduced to-20 ℃, from test specimen tube, take out agitator, the sample on agitator is recovered to test specimen tube.From cartridge filter, take out strainer, put into the sample of test specimen tube, the suction filtration mouth of strainer connects pumping and filtering device.Open pumping and filtering device, carry out suction filtration.When sample liquid level approaches strainer, then add solvent 200ml, continue suction filtration.Reclaim suction filtration liquid and filter cake.
(1), reclaim the solvent in filtrate and filter cake, obtain slack wax and pressed oil, calculate the yield of slack wax and pressed oil.
Experiment is carried out respectively by three different experiments personnel, the yield data of contrast slack wax and pressed oil:
| Project | 1 | 2 | 3 |
| Use equipment | The present invention | The present invention | The present invention |
| Oil product yield % | 78.30 | 78.28 | 78.32 |
| Slack wax yield % | 21.70 | 21.72 | 21.68 |
From upper table, testing data can be found out, adopts experimental technique of the present invention, and three oil product yield experimental results are that 78.30% 3 slack wax yield experimental result is 21.70% ± 0.02%.Three times experimental result fluctuation range is ± 0.02%, possesses good consistence and collimation between data.
Contrast experiment
Experiment oil product: deasphalted oil;
Solvent: toluene and 2-butanone mixture, volume ratio is 1:1;
Agent-oil ratio: about 6:1;
Above-mentioned experiment oil product is identical with embodiment 1 source, all takes from same sample; Solvent is all taken from same solvent samples; Three experimenters that experiment continues in embodiment 1 carry out respectively.
Experimental installation: original solvents dewaxing device
Experimentation: first configure solvent, add respectively 750ml toluene and 750ml2-butanone in 2L graduated cylinder, fully stir, mix standby;
The solvent that measures 400ml is preheating to 40 ℃ in water-bath;
Take sample oil product 200.0g, join in solvent dewaxing equipment test specimen tube, in water-bath, be heated to 40 ℃, add the solvent 400ml that is preheating to 40 ℃, stir sample is dissolved completely;
Open solvent dewaxing equipment, cryostat temperature is set and is-25 ℃, start refrigeration;
Test specimen tube is taken out from water-bath, dry water, be placed in solvent dewaxing equipment;
Residual solvent is collected in airtight bottle, be placed into refrigerator freezing standby.When specimen temperature drops to room temperature, manually in refrigerator, take out solvent, start to add solvent.Add 200ml at every turn, add altogether 3 times.In adition process, constantly stir sample, observe sample cooling temperature, intermittent stirring sample.When sample, solvent, filter temperature are all reduced to-20 ℃, from test specimen tube, take out agitator, the sample on agitator is recovered to test specimen tube.From cartridge filter, take out strainer, put into the sample of test specimen tube, the suction filtration mouth of strainer connects pumping and filtering device.Open pumping and filtering device, carry out suction filtration.When sample liquid level approaches strainer, then add solvent 200ml, continue suction filtration.
Reclaim suction filtration liquid and filter cake.Reclaim the solvent in filtrate and filter cake, obtain slack wax and pressed oil, calculate the yield of slack wax and pressed oil.
The yield data of contrast slack wax and pressed oil:
| Project | 4 | 5 | 6 |
| Use equipment | Original device | Original device | Original device |
| Oil product yield % | 78.90 | 77.50 | 78.50 |
| Slack wax yield % | 21.10 | 22.50 | 21.50 |
From upper table, testing data can be found out, adopts the experimental technique of original device, between three oil product yields and three slack wax yield experimental results, all has larger difference, and data fluctuations scope is 1.0%-1.4%.
(2), in above-mentioned experimentation, we adopt same procedure and the same terms to monitor respectively to solvent evaporates related data respectively, measured data contrast situation:
While adopting the inventive method to carry out above-mentioned experiment, constantly monitor toluene concentration in the air of test specimen tube top, monitoring data mean value is as follows:
| Monitoring time | While adding solvent | In whipping process | In suction filtration process |
| Use equipment | The present invention | The present invention | The present invention |
| Toluene concentration mg/m in air 3 | 20 | 20 | 25 |
While testing in ventilating kitchen, three main experimental phase operator fail obviously to feel have toluene smell substantially;
Measured data shows, airborne toluene concentration does not surpass 25mg/m all the time
3.
While adopting original device to carry out above-mentioned experiment, constantly monitor toluene concentration in the air of test specimen tube top, monitoring data mean value is as follows:
| Monitoring time | While adding solvent | In whipping process | In suction filtration process |
| Use equipment | Original device | Original device | Original device |
| Toluene concentration mg/m in air 3 | 70 | 60 | 45 |
While testing in ventilating kitchen, three main experimental phase operator all obviously feel that toluene smell is denseer, need to wear gas mask.
Measured data also proves, three main experimental phase toluene concentration are respectively apparently higher than the measured data of embodiment 1.
In experimentation, the large reason of toluene volatilization quantity is, in experimentation solvent repeatedly add, the process such as sample suction filtration, need pick and place respectively solvent drum, test specimen tube; And, the joint effect of the serial factors such as steam output increase that when solvent is toppled over, the impact of liquid stream and envrionment temperature are brought.
(3), the time statistical conditions contrast of experiment operator experiment whole process solvent contact:
The present invention:
In experimentation, in experimental period and experimental project, experimenter's solvent contact time adds up as follows:
| Project | 1 | 2 | 3 |
| Use equipment | The present invention | The present invention | The present invention |
| Integral experiment time min | 120 | 120 | 125 |
| Experimenter's solvent contact time min | 5 | 5 | 5 |
In experimentation, experimenter's solvent contact time is 5 minutes, is solvent setup time and time of solvent being added to solvent drum and cartridge filter.
The simultaneous test of original device:
In experimentation, in experimental period and experimental project, experimenter's solvent contact time adds up as follows:
| Project | 4 | 5 | 6 |
| Use equipment | Original device | Original device | Original device |
| Integral experiment time min | 150 | 155 | 153 |
| Experimenter's solvent contact time min | 18 | 20 | 19 |
In experimentation, experimenter's multiple-contact solvent, is 18-20 minute owing to all needing manually to add solvent, the time span of solvent contact in sample at every turn.
Second group of contrast experiment:
Experiment oil product: decompressed wax oil;
Solvent: toluene and 2-butanone mixture, volume ratio is 4:6;
Agent-oil ratio: about 4:1;
Experimental installation: solvent dewaxing equipment of the present invention
Experimentation: first configure solvent, add respectively 400ml toluene and 600ml2-butanone in 2L graduated cylinder, fully stir, mix standby;
The solvent that measures 200ml is preheating to 40 ℃ in water-bath;
Take sample oil product 200.0g, join in solvent dewaxing equipment test specimen tube, in water-bath, be heated to 40 ℃, add the solvent 200ml that is preheating to 40 ℃, stir sample is dissolved completely;
Open solvent dewaxing equipment, cryostat temperature is set and is-25 ℃, start refrigeration;
Test specimen tube is taken out from water-bath, dry water, be placed in solvent dewaxing equipment;
Residual solvent is added respectively to solvent drum and cartridge filter, and solvent drum adds solvent 700ml, and cartridge filter adds solvent 100ml, and strainer is put into cartridge filter, builds each cover plate;
When specimen temperature drops to room temperature, start to add solvent.Add 200ml at every turn, add altogether 2 times.In adition process, constantly stir sample, observe sample cooling temperature, intermittent stirring sample.When sample, solvent, filter temperature are all reduced to-20 ℃, from test specimen tube, take out agitator, the sample on agitator is recovered to test specimen tube.From cartridge filter, take out strainer, put into the sample of test specimen tube, the suction filtration mouth of strainer connects pumping and filtering device.Open pumping and filtering device, carry out suction filtration.When sample liquid level approaches strainer, then add solvent 200ml, continue suction filtration.Reclaim suction filtration liquid and filter cake.
(1), reclaim the solvent in filtrate and filter cake, obtain slack wax and pressed oil, calculate the yield of slack wax and pressed oil.
Experiment is carried out respectively by three different experiments personnel, the yield data of contrast slack wax and pressed oil:
| Project | 1 | 2 | 3 |
| Use equipment | The present invention | The present invention | The present invention |
| Oil product yield % | 76.82 | 76.79 | 76.84 |
| Slack wax yield % | 23.18 | 23.21 | 23.16 |
From upper table, testing data can be found out, adopts experimental technique of the present invention, and three oil product yield experimental results are that 76.815% ± 0.025%, three slack wax yield experimental results are 23.185% ± 0.025%.The fluctuation range of three experimental results is ± 0.025%, possesses good consistence and collimation between data.
Contrast experiment
Experiment oil product: decompressed wax oil;
Solvent: toluene and 2-butanone mixture, volume ratio is 4:6;
Agent-oil ratio: about 4:1;
Above-mentioned experiment oil product is identical with embodiment 1 source, all takes from same sample; Solvent is all taken from same solvent samples; Three experimenters that experiment continues in embodiment 1 carry out respectively.
Experimental installation: original solvents dewaxing device
Experimentation: first configure solvent, add respectively 400ml toluene and 600ml2-butanone in 2L graduated cylinder, fully stir, mix standby;
The solvent that measures 200ml is preheating to 40 ℃ in water-bath;
Take sample oil product 200.0g, join in solvent dewaxing equipment test specimen tube, in water-bath, be heated to 40 ℃, add the solvent 200ml that is preheating to 40 ℃, stir sample is dissolved completely;
Open solvent dewaxing equipment, cryostat temperature is set and is-25 ℃, start refrigeration;
Test specimen tube is taken out from water-bath, dry water, be placed in solvent dewaxing equipment;
Residual solvent is collected in airtight bottle, be placed into refrigerator freezing standby.When specimen temperature drops to room temperature, manually in refrigerator, take out solvent, start to add solvent.Add 200ml at every turn, add altogether 2 times.In adition process, constantly stir sample, observe sample cooling temperature, intermittent stirring sample.When sample, solvent, filter temperature are all reduced to-20 ℃, from test specimen tube, take out agitator, the sample on agitator is recovered to test specimen tube.From cartridge filter, take out strainer, put into the sample of test specimen tube, the suction filtration mouth of strainer connects pumping and filtering device.Open pumping and filtering device, carry out suction filtration.When sample liquid level approaches strainer, then add solvent 200ml, continue suction filtration.
Reclaim suction filtration liquid and filter cake.Reclaim the solvent in filtrate and filter cake, obtain slack wax and pressed oil, calculate the yield of slack wax and pressed oil.
The yield data of contrast slack wax and pressed oil:
| Project | 4 | 5 | 6 |
| Use equipment | Original device | Original device | Original device |
| Oil product yield % | 76.75 | 77.67 | 75.88 |
| Slack wax yield % | 23.25 | 22.33 | 24.12 |
From upper table, testing data can be found out, adopts the experimental technique of original device, between three oil product yields and three slack wax yield experimental results, all has larger difference, and data fluctuations scope is 0.87%-1.79%.
(2), the time statistical conditions contrast of experiment operator experiment whole process solvent contact:
The present invention:
In experimentation, in experimental period and experimental project, experimenter's solvent contact time adds up as follows:
| Project | 1 | 2 | 3 |
| Use equipment | The present invention | The present invention | The present invention |
| Integral experiment time min | 120 | 120 | 125 |
| Experimenter's solvent contact time min | 5 | 5 | 5 |
In experimentation, experimenter's solvent contact time is 5 minutes, is solvent setup time and time of solvent being added to solvent drum and cartridge filter.
The simultaneous test of original device:
In experimentation, in experimental period and experimental project, experimenter's solvent contact time adds up as follows:
| Project | 4 | 5 | 6 |
| Use equipment | Original device | Original device | Original device |
| Integral experiment time min | 150 | 155 | 153 |
| Experimenter's solvent contact time min | 18 | 17 | 19 |
In experimentation, experimenter's multiple-contact solvent, is 17-19 minute owing to all needing manually to add solvent, the time span of solvent contact in sample at every turn.
Claims (3)
1. hydrocarbon ils dewaxing laboratory apparatus, it comprises main body frame, controller with digital display screen is installed in main body frame, liftable agitator, miniature volume pump, cryostat, test specimen tube, and pumped vacuum systems and refrigeration system outside device, wherein, pumped vacuum systems is connected with strainer, cryostat access refrigeration system refrigeration, liftable agitator be arranged on test specimen tube directly over, it is characterized in that, described experiment solvent dewaxing laboratory apparatus also includes solvent injected system, solvent drum, cartridge filter, described solvent injected system is by the miniature volume pump being controlled by the controller, T-valve and pipeline form, described miniature metering pump intake piping road is connected with described solvent drum, described T-valve is arranged on described miniature metering pump discharge pipe road, two exit end of described T-valve are connected with solvent drum with described test specimen tube respectively by pipeline, when described test specimen tube and described solvent drum and the work of described cartridge filter, be placed in cryostat simultaneously, described test specimen tube, solvent drum is respectively arranged with cartridge filter the temperature sensor being connected with digital display screen,
Described solvent drum, cartridge filter are consistent with the scantlings of the structure of described test specimen tube, possess interchangeability;
On described solvent drum, cartridge filter and described test specimen tube cylinder circle, be provided with pilot hole, by steady brace, be positioned on board panel;
The volume of the group/external member of described solvent drum, cartridge filter and test specimen tube be one group/cover or many groups/cover, volume between each group/external member is different.
2. hydrocarbon ils dewaxing laboratory apparatus as claimed in claim 1, is characterized in that, group/kit size specification of described not isometric solvent drum, cartridge filter, test specimen tube is 0.5～5 liter.
3. an experimental technique that adopts hydrocarbon ils dewaxing laboratory apparatus as claimed in claim 1, comprises the following steps:
Preparation solvent preheating in water-bath; Take sample, join in solvent dewaxing equipment test specimen tube, in water-bath, heat, add the solvent of preheating and stir sample is dissolved completely;
Test specimen tube is taken out from water-bath, dry water and be placed in solvent dewaxing equipment; Open solvent dewaxing equipment, cryostat temperature is set, start refrigeration;
Residual solvent is added respectively to solvent drum and cartridge filter, strainer is put into cartridge filter, build each cover plate;
When specimen temperature drops to room temperature, start to add solvent according to test requirements document gradation; In solvent adition process, constantly stir sample;
After solvent has added, observe sample cooling temperature, intermittent stirring sample;
When the temperature of the sample in test specimen tube, the solvent in solvent drum and strainer is all reduced to design temperature, from test specimen tube, take out agitator, the sample on agitator is recovered to test specimen tube;
From cartridge filter, take out strainer, put into the sample of test specimen tube, open pumping and filtering device, carry out suction filtration;
When sample liquid level approaches strainer, then add solvent, continue suction filtration;
Reclaim the solvent in filtrate and filter cake, obtain slack wax and pressed oil.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1521242A (en) * | 2003-01-30 | 2004-08-18 | 中国石油化工股份有限公司 | Auxiliary test device for solvent dewaxing |
| CN202346976U (en) * | 2011-11-09 | 2012-07-25 | 上海继润石化科技有限公司 | Novel device for processing urea by adopting dewaxing dry method |
| CN202658137U (en) * | 2012-06-07 | 2013-01-09 | 中国石油化工股份有限公司 | Solvent dewaxing device |
| JP5414404B2 (en) * | 2009-07-21 | 2014-02-12 | 大崎電気工業株式会社 | Coil for standard voltage measurement of watt-hour meter |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US553564A (en) * | 1896-01-28 | Corn-harvester | ||
| TWI513811B (en) * | 2011-10-27 | 2015-12-21 | Hon Hai Prec Ind Co Ltd | Device for automatically removing wax |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1521242A (en) * | 2003-01-30 | 2004-08-18 | 中国石油化工股份有限公司 | Auxiliary test device for solvent dewaxing |
| JP5414404B2 (en) * | 2009-07-21 | 2014-02-12 | 大崎電気工業株式会社 | Coil for standard voltage measurement of watt-hour meter |
| CN202346976U (en) * | 2011-11-09 | 2012-07-25 | 上海继润石化科技有限公司 | Novel device for processing urea by adopting dewaxing dry method |
| CN202658137U (en) * | 2012-06-07 | 2013-01-09 | 中国石油化工股份有限公司 | Solvent dewaxing device |
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Address after: 100010 room 1414, Hai Yuan building, 25 Chaoyangmen North Street, Dongcheng District, Beijing. Co-patentee after: CNOOC OIL & PETROCHEMICALS Co.,Ltd. Patentee after: CHINA NATIONAL OFFSHORE OIL Corp. Co-patentee after: CNOOC RESEARCH INSTITUTE OF REFINING AND PETROCHEMICALS (BEIJING) Co.,Ltd. Address before: 100010 Chaoyangmen North Street, Dongcheng District, Dongcheng District, Beijing Co-patentee before: CNOOC OIL & PETROCHEMICALS Co.,Ltd. Patentee before: CHINA NATIONAL OFFSHORE OIL Corp. Co-patentee before: CNOOC RESEARCH INSTITUTE OF REFINING AND PETROCHEMICALS (BEIJING) Co.,Ltd. |
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Effective date of registration: 20180511 Address after: 100010 room 1414, Hai Yuan building, 25 Chaoyangmen North Street, Dongcheng District, Beijing. Co-patentee after: CNOOC OIL & PETROCHEMICALS Co.,Ltd. Patentee after: CHINA NATIONAL OFFSHORE OIL Corp. Co-patentee after: CNOOC RESEARCH INSTITUTE OF REFINING AND PETROCHEMICALS (BEIJING) Co.,Ltd. Co-patentee after: CNOOC (QINGDAO) HEAVY OIL PROCESSING ENGINEERING TECHNOLOGY RESEARCH CENTER Co.,Ltd. Address before: 100010 room 1414, Hai Yuan building, 25 Chaoyangmen North Street, Dongcheng District, Beijing. Co-patentee before: CNOOC OIL & PETROCHEMICALS Co.,Ltd. Patentee before: CHINA NATIONAL OFFSHORE OIL Corp. Co-patentee before: CNOOC RESEARCH INSTITUTE OF REFINING AND PETROCHEMICALS (BEIJING) Co.,Ltd. |