CN103837423A - Device for simultaneously measuring plurality of types of insoluble substances - Google Patents
Device for simultaneously measuring plurality of types of insoluble substances Download PDFInfo
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- CN103837423A CN103837423A CN201410111336.5A CN201410111336A CN103837423A CN 103837423 A CN103837423 A CN 103837423A CN 201410111336 A CN201410111336 A CN 201410111336A CN 103837423 A CN103837423 A CN 103837423A
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- insolubles
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Abstract
The invention discloses a device for simultaneously measuring a plurality of types of insoluble substances. The device comprises more than two insoluble substance determining devices, a vacuum pump and a solvent system, wherein the insoluble substance determining devices comprise a first insoluble substance determining device or a second insoluble substance determining device; each insoluble substance determining device comprises a heating device, a liquid feeding device, a pumping device and a solvent room; the insoluble substance determining devices are arranged in the shells; the solvent system is connected with the pumping device by a liquid feeding pipeline; the pumping device of the first insoluble substance determining device further comprises a steam loop; the solvent system is connected with the solvent room of the first insoluble substance determining device by the liquid feeding pipeline; the second insoluble substance determining device further comprises a sealing piece; the sealing piece is provided with an agitating device and a liquid inlet; the liquid inlet is connected with the solvent system by a pipeline. According to the device disclosed by the invention, a set of peripheral device is commonly utilized to carry out insoluble substance determination of the two types of insoluble substances, so as to simultaneously determine toluene quinoline insoluble substances.
Description
Technical field
The invention belongs to instrumental analysis field, be specifically related to the integrated device that a kind of insolubles is measured.
Background technology
The purposes difference of pitch, they are also different to the requirement of asphalt quality.In this area, general normal use benzene insoluble (T.I) and two indexs of quinoline insolubles (Q.I) are evaluated the combination property of pitch.Carbon electrode and refractory industry, be all used as coal tar pitch cementing agent and impregnant, and when it is when the cementing agent, the residual degree of coke of the contained form in carbon of coal-tar asphalt is high as far as possible.
The toluene carrying out for pitch at present and the assay method of quinoline insolubles, all need to have used two cover experimental provisions, and in experimentation, be to need operating personnel's Long contact time toxic gas, and operating personnel's health of human body has been caused to very large harm.
Summary of the invention
The gas leakage and the manual defect of needs that occur when measuring insolubles in prior art, the invention provides a kind of device of simultaneously measuring polymorphic type insolubles, described device comprises plural insolubles determinator, vacuum pump and solvent system, described insolubles determinator is the first insolubles determinator or the second insolubles determinator, described insolubles determinator includes heating arrangement, liquid-adding device, extractor and solvent compartment, described insolubles determinator is all arranged in housing, described housing is connected with vacuum pump, described solvent system is connected with extractor by charging line,
The extractor of described the first insolubles determinator also comprises steam-return line, and described solvent system is connected with the solvent compartment of the first insolubles determinator by charging line; This type of extractor that contains steam-return line and siphon suction filtering tube can be for the mensuration of toluene insolubles.
The extractor of described the second insolubles determinator is connected by funnel with solvent compartment, and described the second insolubles determinator extractor is not containing steam-return line.
Preferably, the extractor of described insolubles determinator is provided with siphon suction filtering tube, and the inlet of described siphon suction filtering tube is arranged on extractor bottom position, guarantees that discharge opeing is thorough, and described siphonal height is lower than dissolving liquid level.
Device of the present invention can be the first or second insolubles determinator, also can comprise that stream oriented device is to realize several functions simultaneously simultaneously.Above-mentioned housing can be discrete or same housing.
Preferred, described the first insolubles determinator also comprises the first cylinder and condenser pipe, and described condenser pipe is connected with the first cylinder, and carries out lifting by it, and described condenser pipe is connected with the extractor of the first insolubles determinator.
Preferred, on described steam-return line, be also provided with drying heater, outside the solvent compartment of described the first insolubles determinator, be also provided with solvent heater.
Preferably, described the second insolubles determinator also comprises a seal, is provided with stirring apparatus and inlet on described seal, and described inlet is connected with solvent system by pipeline.
Preferred, the leakage fluid dram of the siphon suction filtering tube of the extractor of described the second insolubles determinator is arranged at the middle and upper part of funnel.
Preferred, described the second insolubles determinator also comprises a seal, is provided with stirring apparatus and inlet on described seal, and described inlet is connected with solvent system by pipeline.
Preferred, the bottom of described the second insolubles determinator is connected with the 3rd cylinder.Bottom herein can be solvent compartment, or the integrative-structure of funnel and solvent compartment's formation.
Preferred, the bottom of the extractor of described the second insolubles determinator and funnel place are respectively arranged with heating arrangement.
Preferred, the solvent compartment of described insolubles determinator is connected with waste collecting device by pipeline.
This device can be used for detection of coal-tar pitch, modified pitch, coal asphalt oil for building up highway, wood preserving oil and carbon black the test of toluene, quinoline insolubles in coking raw material oil, and completely cut off in experimentation the harmful gas producing when the heating owing to adding hot toluene and quinoline, ensure operating personnel's personal safety.This device adopts Programmable Logic Controller PLC to control, and realizes whole automation of motions.Mainly comprise: process, the vacuum such as the pre-heating system of solution, liquid feeding, heating, stirring, filtration.
The present invention carries out insolubles mensuration to two class insolubless by public a set of peripheral unit simultaneously, when can realizing toluene and quinoline insolubles, measures.
In the time of toluene insolubles determination experiment, multi-pipeline can be set, add liquid mouth structure, utilize the lifting of cylinder and decline to realizing and put filter paper and opening sealing, carry out in real time vacuumizing in the seal hatch of storehouse, prevent the diffusion of toxic gas in experimentation, ensured operating personnel's health of human body.
In the time of quinoline insolubles determination test, utilize stirring rod as weighing carrier and add dissolving indoor on sample, the Transfer Error of avoiding other method all to exist.At top seal parts, place has added input duct, can realize in experimentation the function of liquid feeding at any time; In dissolving side, chamber, siphon suction filtering tube is set, and makes siphon suction filtering tube siphon height dissolve indoor height higher than solution; Install heater element additional in dissolving outdoor, can be in quinoline insolubles determination experiment thermal source is provided.
The present invention all adopts gas-powered aspect control, avoids the generation of static, can play explosion-proof; Adopt the control of external electromagnetic valve, can realize robotization control.
Brief description of the drawings
The device schematic diagram of Fig. 1, insolubles determinator.
The control schematic diagram of Fig. 2, apparatus of the present invention.
Accompanying drawing mark:
1, condenser pipe; 2, extractor; 3, filtration paper cylinder; 4, sample; 5, flux bin; 6, well heater; 7, the first cylinder; 8, drying heater; 10, seal; 11, air motor; 12, paddle; 13, sample; 14, the second cylinder; 15, primary heater; 16, the second extractor; 17, secondary heater; 18, filter paper; 19, H funnel; 20, the second solvent compartment; 21, the 3rd cylinder; 22, waste liquid barrel; 23, shell.
Embodiment
Referring to Fig. 1, can measure the experimental provision of toluene and quinoline insolubles simultaneously, comprise insolubles determinator, vacuum pump and the solvent system of two, described insolubles determinator is respectively toluene insoluble object measuring device or quinoline non-soluble object measuring device, described insolubles determinator is all arranged in housing 23 and 24, described housing 23 is connected with vacuum pump with 24, and described solvent system is connected with extractor 2,16 by charging line.
Referring to Fig. 2, device of the present invention can also configure PLC master controller, realizes the control for well heater, well heater, cylinder, solenoid valve and vacuum pump by it.
Toluene insoluble object measuring device comprises condenser pipe 1, extractor 2, solvent compartment 5, well heater 6, drying heater 8, steam-return line and the first cylinder 7, described drying heater 6 is arranged on steam-return line, the bottom of described solvent compartment 5 is connected with waste liquid device by pipeline, described the first cylinder 7 can be realized the lifting of condenser pipe 1, and then can put into filtration paper cylinder 3 and sample 4, described condenser pipe is connected with the extractor of the first insolubles determinator, can realize the sealing for system.Extractor 2 is provided with siphon suction filtering tube, and the inlet of described siphon suction filtering tube is arranged on extractor bottom position, guarantees that discharge opeing is thorough, and described siphonal height is lower than dissolving liquid level.
While measuring toluene insolubles, can carry out as follows:
1) make filtration paper cylinder: diameter 125mm middling speed quantitative filter paper is converted into external diameter 44mm filtration paper cylinder, filtration paper cylinder is soaked in toluene after 24 hours and take out, dry, be placed in measuring cup, for subsequent use after 115-120 DEG C of drying box inner drying.
2) weigh a certain amount of sample, place in dried filtration paper cylinder.
3) lifting cylinder, is promoted to certain altitude by condenser pipe.
4) open form door, weighted filtration paper cylinder is slowly put into extractor, filtration paper cylinder bottom and extractor bottom are developed.
5) close form door, lifting cylinder declines, by ground under condenser pipe and the sealing of extracting barrel upper grinding port.
6) start pipeline heater, start liquid-adding device a certain amount of toluene is added in flux bin.
7) heater, unlatching condensate water, unlatching vacuum pump.
8) extraction times or the extraction time equipment set by equipment extract automatically.
10) extracted toluene liquid automatic-discharging in rear flask to waste liquid barrel.
11) start drying heater, filter paper is dried to 20-60min.
12) air cylinder lifting, equipment carries out auditory tone cues experiment and finishes.
13) take out filter paper bucket and be dried, weigh, calculate insolubles content.
Quinoline non-soluble object measuring device comprises seal 10, air motor 11, paddle 12, sample 13, the second cylinder 14, primary heater 15, the second extractor 16, secondary heater 17, filter paper 18, H funnel 19, the 3rd cylinder 21 and the second solvent compartment 20.Wherein on seal 10, be provided with inlet, it is connected with solvent compartment by input duct, is also provided with stirring apparatus on it, can realize the weighing for sample by the blade of stirring arm 12.The second cylinder 14 can be realized lifting and the decline for seal 10.
Quinoline non-soluble object measuring device does not comprise steam-return line, and the second extractor 16 is connected by H funnel 19 with the second solvent compartment, the outer heating arrangement that is provided with of the bottom of the second extractor 16 and H funnel 19.The second solvent compartment 20 is connected with waste liquid recovery apparatus by pipeline.The extractor of quinoline is provided with siphon suction filtering tube, and its inlet is arranged on and dissolves chamber bottom position, guarantees that discharge opeing is thorough.Leakage fluid dram is arranged on H funnel 19 top placed in the middle, guarantees that liquid flows into filter paper centre.Siphon suction filtering tube should be arranged on certain altitude, guarantees can not occur siphonic effect in the time that stirring and dissolving is carried out in experiment.In the time that needs filter, can make solution carry out suction filtration via siphon suction filtering tube inflow filter paper middle part by switching vacuum pump.
While measuring quinoline insolubles, can be undertaken by following step:
1) filter paper is placed in toluene soak 24 hours take out dry, dry after for subsequent use.
2) filter paper after drying is converted into filtration paper cylinder and places measuring cup weighing.
3) stirring rod in quinoline storehouse is dried to rear weighing.
4) take a certain amount of sample with the paddle after drying as carrier.
5) the 3rd cylinder declines, and takes out funnel, and the filtration paper cylinder folding is placed in funnel.
6) funnel is placed to suction filtration bucket upper port, the 3rd cylinder rises.
7) the second air cylinder lifting, to certain altitude, is arranged on stirring apparatus lower end interface by load weighted burnt grain.
8) near upper and lower both ends of the surface sealing under the second cylinder
9) close form door, start pipe heating device, start liquid-adding device, a certain amount of quinoline is heated to design temperature and is added in extracting barrel by pipe heating device.
10) vacuum pump is opened.
11) start well heater, heated at constant temperature.
12) start stirring apparatus, frequently stir.
13) after 30 minutes, stir and stop, vacuum pump switches to suction filtration pipeline.
14) liquid is drawn to and in filtration paper cylinder, is carried out suction filtration by U trap by vacuum pump.
15) start liquid-adding device, repeatedly rinse extracting barrel and carry out suction filtration with a certain amount of toluene and quinoline.
16) suction filtration finishes rear suction filtration liquid in bucket and automatically drains into exhausted bath box.
17) vacuum pump switches to pump-line, the second air cylinder lifting.
18) start well heater filter paper is carried out to drying and processing.
19) after drying, the 3rd cylinder declines.
20) filter paper bucket is taken out, weighs, calculates from funnel insolubles content.
Said apparatus can be realized the mensuration of toluene and quinoline insolubles, clearly, toluene insoluble object measuring device can be replaced into quinoline non-soluble object measuring device, and quinoline non-soluble object measuring device can be replaced into toluene insoluble object measuring device, when it can realize two samples, measures.
Claims (10)
1. measure the device of polymorphic type insolubles for one kind simultaneously, it is characterized in that, described device comprises plural insolubles determinator, vacuum pump and solvent system, described insolubles determinator is the first insolubles determinator or the second insolubles determinator, described insolubles determinator includes heating arrangement, liquid-adding device, extractor and solvent compartment, described insolubles determinator is all arranged in housing, described housing is connected with vacuum pump, and described solvent system is connected with extractor by charging line;
The extractor of described the first insolubles determinator also comprises steam-return line, and described solvent system is connected with the solvent compartment of the first insolubles determinator by charging line;
The extractor of described the second insolubles determinator is connected by funnel with solvent compartment.
2. device according to claim 1, it is characterized in that, the extractor of described insolubles determinator is provided with siphon suction filtering tube, and the inlet of described siphon suction filtering tube is arranged on extractor bottom position, guarantee that discharge opeing is thorough, described siphonal height is lower than dissolving liquid level.
3. device according to claim 1 and 2, it is characterized in that, described the first insolubles determinator also comprises the first cylinder and condenser pipe, and described condenser pipe is connected with the first cylinder, and carrying out lifting by it, described condenser pipe is connected with the extractor of the first insolubles determinator.
4. device according to claim 1 and 2, is characterized in that, is also provided with drying heater on described steam-return line, is also provided with solvent heater outside the solvent compartment of described the first insolubles determinator.
5. device according to claim 1 and 2, is characterized in that, described the second insolubles determinator also comprises a seal, is provided with stirring apparatus and inlet on described seal, and described inlet is connected with solvent system by pipeline.
6. device according to claim 2, is characterized in that, the leakage fluid dram of the siphon suction filtering tube of the extractor of the second insolubles determinator is arranged at the middle and upper part of funnel.
7. device according to claim 1 and 2, is characterized in that, the bottom of described the second insolubles determinator is connected with the 3rd cylinder.
8. device according to claim 1 and 2, is characterized in that, the bottom of the extractor of described the second insolubles determinator and funnel place are respectively arranged with heating arrangement.
9. device according to claim 1 and 2, is characterized in that, the solvent compartment of described insolubles determinator is connected with waste collecting device by pipeline.
10. device according to claim 1 and 2, is characterized in that, the stirring apparatus of described the second insolubles determinator is provided with stirring vane, the weighing that this stirring vane can carry out sample as carrier and reinforced.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410111336.5A CN103837423B (en) | 2014-03-24 | 2014-03-24 | A kind of device simultaneously measuring polymorphic type insoluble matter |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410111336.5A CN103837423B (en) | 2014-03-24 | 2014-03-24 | A kind of device simultaneously measuring polymorphic type insoluble matter |
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| CN103837423B CN103837423B (en) | 2016-06-15 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458479A (en) * | 2014-12-03 | 2015-03-25 | 宁波检验检疫科学技术研究院 | Device for measuring sediments in crude oil and heavy oil |
| CN108531206A (en) * | 2018-04-03 | 2018-09-14 | 西南石油大学 | A kind of the pyrobitumen high temperature circulation dissolver and method of high evolution |
| CN109540730A (en) * | 2018-12-19 | 2019-03-29 | 北京英斯派克科技有限公司 | A kind of unattended environment-friendly type insolubles content measurement device and method |
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| CN2044255U (en) * | 1988-10-19 | 1989-09-13 | 张虞安 | Purrifying device for bilirubin |
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Patent Citations (4)
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| CN2044255U (en) * | 1988-10-19 | 1989-09-13 | 张虞安 | Purrifying device for bilirubin |
| JPH05264431A (en) * | 1992-01-31 | 1993-10-12 | Ulvac Japan Ltd | Method and apparatus for measuring vapor pressure of sample |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458479A (en) * | 2014-12-03 | 2015-03-25 | 宁波检验检疫科学技术研究院 | Device for measuring sediments in crude oil and heavy oil |
| CN104458479B (en) * | 2014-12-03 | 2017-07-04 | 宁波检验检疫科学技术研究院 | A kind of crude oil and weight oil sediments determine device |
| CN108531206A (en) * | 2018-04-03 | 2018-09-14 | 西南石油大学 | A kind of the pyrobitumen high temperature circulation dissolver and method of high evolution |
| CN108531206B (en) * | 2018-04-03 | 2020-12-29 | 西南石油大学 | High-evolution pyrobitumen high-temperature circulating dissolving device and method |
| CN109540730A (en) * | 2018-12-19 | 2019-03-29 | 北京英斯派克科技有限公司 | A kind of unattended environment-friendly type insolubles content measurement device and method |
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| CN103837423B (en) | 2016-06-15 |
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