CN103837423B - A kind of device simultaneously measuring polymorphic type insoluble matter - Google Patents
A kind of device simultaneously measuring polymorphic type insoluble matter Download PDFInfo
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- CN103837423B CN103837423B CN201410111336.5A CN201410111336A CN103837423B CN 103837423 B CN103837423 B CN 103837423B CN 201410111336 A CN201410111336 A CN 201410111336A CN 103837423 B CN103837423 B CN 103837423B
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Abstract
The invention discloses a kind of device simultaneously measuring polymorphic type insoluble matter, described device includes plural insoluble matter determinator, vacuum pump and solvent system, insoluble matter determinator is the first insoluble matter determinator or the second insoluble matter determinator, insoluble matter determinator all includes heater, liquid-adding device, extractor and solvent compartment, insoluble matter determinator may be contained within housing, and solvent system is connected by charging line and extractor; The extractor of the first insoluble matter determinator also includes steam-return line, and solvent system is connected by the solvent compartment of charging line and the first insoluble matter determinator; Second insoluble matter determinator also includes a sealing member, and sealing member is provided with agitating device and inlet, and inlet is connected by pipeline and solvent system. Two class insoluble matters are carried out insoluble matter mensuration by public a set of peripheral unit by the present invention simultaneously, it is possible to achieve toluene and mensuration while quinoline insolubles.
Description
Technical field
The invention belongs to Instrumental Analysis field, be specifically related to the integrated device that a kind of insoluble matter measures.
Background technology
The purposes of Colophonium is different, and they are also different to the requirement of asphalt quality. In this area, generally often use benzene insoluble (T.I) and two indexs of quinoline insolubles (Q.I) to evaluate the combination property of Colophonium. Carbon electrode and refractory industry, be all used as binding agent and impregnating agent by coal tar pitch, and when it is used as binding agent, the coke residual degree in the form of carbon contained by coal tar asphalt is high as far as possible.
The toluene carried out currently for Colophonium and the assay method of quinoline insolubles, all need to have used two set experimental provisions, and be need operator's Long contact time toxic gas in experimentation, the health of human body of operator is caused very big harm.
Summary of the invention
For in prior art measure insoluble matter time occur gas leakage and need manual defect, the invention provides a kind of device simultaneously measuring polymorphic type insoluble matter, described device includes plural insoluble matter determinator, vacuum pump and solvent system, described insoluble matter determinator is the first insoluble matter determinator or the second insoluble matter determinator, described insoluble matter determinator all includes heater, liquid-adding device, extractor and solvent compartment, described insoluble matter determinator may be contained within housing, described housing and vacuum pump connect, described solvent system is connected by charging line and extractor,
The extractor of described first insoluble matter determinator also includes steam-return line, and described solvent system is connected by the solvent compartment of charging line and the first insoluble matter determinator;This type of extractor containing steam-return line and siphon suction filtering tube may be used for the mensuration of toluene insolubles.
Extractor and the solvent compartment of described second insoluble matter determinator are connected by funnel, and described second insoluble matter determinator extractor is without steam-return line.
Preferably, the extractor of described insoluble matter determinator is provided with siphon suction filtering tube, and the inlet of described siphon suction filtering tube is arranged on extractor bottom position, it is ensured that discharge opeing is thorough, and described siphonal height is lower than dissolving liquid level.
Assembly of the invention can be the first or second insoluble matter determinator, it is also possible to include stream oriented device to realize several functions simultaneously simultaneously. Above-mentioned housing can be discrete or same housing.
Connecting it is furthermore preferred that described first insoluble matter determinator also includes the first cylinder and condensing tube, described condensing tube and the first cylinder, and lifted by it, the extractor of described condensing tube and the first insoluble matter determinator connects.
It is furthermore preferred that described steam-return line is additionally provided with drying heater, outside the solvent compartment of described first insoluble matter determinator, it is additionally provided with solvent heater.
Preferably, described second insoluble matter determinator also includes a sealing member, and described sealing member is provided with agitating device and inlet, and described inlet is connected by pipeline and solvent system.
It is furthermore preferred that the leakage fluid dram of the siphon suction filtering tube of the extractor of described second insoluble matter determinator is arranged at the middle and upper part of funnel.
It is furthermore preferred that described second insoluble matter determinator also includes a sealing member, described sealing member being provided with agitating device and inlet, described inlet is connected by pipeline and solvent system.
It is furthermore preferred that the bottom of described second insoluble matter determinator is connected with the 3rd cylinder. Bottom herein can be solvent compartment, or the integrative-structure that funnel and solvent compartment are constituted.
It is furthermore preferred that the bottom of the extractor of described second insoluble matter determinator and funnel place are respectively arranged with heater.
It is furthermore preferred that the solvent compartment of described insoluble matter determinator is connected by pipeline and waste collecting device.
This device may be used for the test of toluene, quinoline insolubles in detection coal tar pitch, modified coal tar pitch, coal asphalt oil for building up highway, coal-tar creosote solution and white carbon black coking raw material oil, and completely cut off the harmful gas produced when heating in experimentation due to heating toluene and quinoline, it is ensured that the personal safety of operator. This device adopts programmable controller PLC to control, it is achieved all automation of motions. Specifically include that process, the vacuum such as the pre-heating system of solution, liquid feeding, heating, stirring, filtration.
Two class insoluble matters are carried out insoluble matter mensuration by public a set of peripheral unit by the present invention simultaneously, it is possible to achieve toluene and mensuration while quinoline insolubles.
When toluene insolubles determination experiment, multi-pipeline, many liquid feedings mouth structure can be set, the lifting and the decline that utilize cylinder realize putting filter paper and opening sealing, carry out carrying out evacuation in the seal hatch of storehouse in real time, prevent the diffusion of toxic gas in experimentation, it is ensured that the health of human body of operator.
When quinoline insolubles determination test, utilize stirring rod as weighing carrier and sample adding dissolving indoor, it is to avoid the Transfer Error that other method all exists. Input duct is added, it is possible to achieve the function of liquid feeding at any time in experimentation at top seal parts place;Siphon suction filtering tube is set dissolving side, room, and makes siphon suction filtering tube siphon height dissolve indoor height higher than solution; Heater element has been installed additional dissolving outdoor, can for quinoline insolubles determination experiment provides thermal source.
The present invention all adopts gas-powered in control, it is to avoid the generation of electrostatic, can play explosion-proof; External electrical magnet valve is adopted to control, it may be achieved Automated condtrol.
Accompanying drawing explanation
Fig. 1, insoluble matter determinator device schematic diagram.
Fig. 2, apparatus of the present invention control schematic diagram.
Accompanying drawing identifies:
1, condensing tube; 2, extractor; 3, filtration paper cylinder; 4, sample; 5, flux bin; 6, heater; 7, the first cylinder; 8, drying heater; 10, sealing member; 11, air motor; 12, stirring 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.
Detailed description of the invention
Referring to Fig. 1, the experimental provision of toluene and quinoline insolubles can be measured simultaneously, including the insoluble matter determinators of two, vacuum pump and solvent system, described insoluble matter determinator respectively toluene insoluble object measuring device or quinoline non-soluble object measuring device, described insoluble matter determinator may be contained within housing 23 and 24, described housing 23 and 24 and vacuum pump connect, described solvent system is connected by charging line and extractor 2,16.
Referring to Fig. 2, assembly of the invention can also configure PLC master controller, by fact referring now to the control of heater, heater, cylinder, electromagnetic valve and vacuum pump.
Toluene insoluble object measuring device includes condensing tube 1, extractor 2, solvent compartment 5, 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 by pipeline and waste liquid device, described first cylinder 7 can realize the lifting of condensing tube 1, and then filtration paper cylinder 3 and sample 4 can be put into, the extractor of described condensing tube and the first insoluble matter determinator connects, it is possible to achieve for the sealing of 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, it is ensured that discharge opeing is thorough, and described siphonal height is lower than dissolving liquid level.
Can carry out as follows when measuring toluene insolubles:
1) make filtration paper cylinder: diameter 125mm middling speed quantitative filter paper is converted into external diameter 44mm filtration paper cylinder, take out after filtration paper cylinder is soaked 24 hours in toluene, dry, be placed in weighing botle, standby after 115-120 DEG C of drying baker inner drying.
2) weigh a certain amount of sample, place in dried filtration paper cylinder.
3) lifting cylinder, is promoted to certain altitude by condensing tube.
4) open form door, weighted filtration paper cylinder is slowly put into extractor, make bottom filtration paper cylinder and develop bottom extractor.
5) closing form door, lifting cylinder declines, and ground under condensing tube and extracting barrel upper grinding port is sealed.
6) start pipeline heater, start liquid-adding device and a certain amount of toluene is added in flux bin.
7) heater, open condensed water, open vacuum pump.
8) extraction times or extraction time equipment by equipment setting extract automatically.
10) toluene liquid automatic-discharging in rear flask has been extracted to waste liquid barrel.
11) start drying heater, filter paper is dried 20-60min.
12) air cylinder lifting, equipment carries out auditory tone cues experiment and terminates.
13) take out filter paper bucket to be dried, weigh, calculate insolubles content.
Quinoline non-soluble object measuring device includes sealing member 10, air motor 11, stirring paddle 12, sample the 13, second cylinder 14, primary heater the 15, second extractor 16, secondary heater 17, filter paper 18, H funnel the 19, the 3rd cylinder 21 and the second solvent compartment 20. Wherein being provided with inlet on sealing member 10, it is connected by input duct and solvent compartment, and it is additionally provided with agitating device, it is possible to realize the weighing for sample by stirring the blade of slurry 12. Second cylinder 14 can realize the lifting for sealing member 10 and decline.
Quinoline non-soluble object measuring device does not include steam-return line, and the second extractor 16 and the second solvent compartment are connected by H funnel 19, are provided with heater outside the bottom of the second extractor 16 and H funnel 19. Second solvent compartment 20 is connected by pipeline and waste liquid recovery apparatus. The extractor of quinoline is provided with siphon suction filtering tube, and its inlet is arranged on dissolving room bottom position, it is ensured that discharge opeing is thorough. Leakage fluid dram is arranged on H funnel 19 top placed in the middle, it is ensured that liquid flows into filter paper centre. Siphon suction filtering tube should be arranged on certain altitude, it is ensured that when experiment is stirred and dissolving, siphonic effect will not occur. When needs are filtered, solution can be made to flow into filter paper middle part via siphon suction filtering tube by switching vacuum pump and carry out sucking filtration.
Can be undertaken by the steps when measuring quinoline insolubles:
1) filter paper is placed in toluene soak 24 hours take out dry, standby after drying.
2) filter paper after drying is converted into filtration paper cylinder and places weighing botle weighing.
3) weigh after the stirring rod in quinoline storehouse being dried.
4) a certain amount of sample is weighed with the paddle after drying as carrier.
5) the 3rd cylinder declines, and takes out funnel, is placed in funnel by the filtration paper cylinder folded.
6) funnel being placed sucking filtration bucket upper port, the 3rd cylinder rises.
7) the second air cylinder lifting is to certain altitude, and load weighted char particle is arranged on agitating device lower end seam.
8) under the second cylinder, near upper and lower both ends of the surface seal
9) close form door, start pipe heating device, start liquid-adding device, a certain amount of quinoline to design temperature and is added in extracting barrel by pipe heating device heating.
10) vacuum pump is opened.
11) heater, heated at constant temperature are started.
12) start agitating device, frequently stir.
13) after 30 minutes, stirring stops, and vacuum pump switches to sucking filtration pipeline.
14) liquid is drawn in filtration paper cylinder by vacuum pump by siphon and carries out sucking filtration.
15) start liquid-adding device, repeatedly rinse extracting barrel with a certain amount of toluene and quinoline and carry out sucking filtration.
16) sucking filtration terminates rear sucking 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 heater and filter paper is carried out drying and processing.
19), after drying, the 3rd cylinder declines.
20) filter paper bucket is taken out from funnel, weighs, calculates insolubles content.
Said apparatus can realize 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, and it measures while can realizing two samples.
Claims (5)
1. the device simultaneously measuring polymorphic type insoluble matter, it is characterized in that, described device includes plural insoluble matter determinator, vacuum pump and solvent system, described insoluble matter determinator includes the first insoluble matter determinator and the second insoluble matter determinator, described insoluble matter determinator all includes heater, liquid-adding device, extractor and solvent compartment, described insoluble matter determinator may be contained within housing, described housing and vacuum pump connect, and described solvent system is connected by charging line and extractor;
The extractor of described first insoluble matter determinator also includes steam-return line, and described solvent system is connected by the solvent compartment of charging line and the first insoluble matter determinator;
Extractor and the solvent compartment of described second insoluble matter determinator are connected by funnel;
The extractor of the described second insoluble matter determinator of the extractor sum of described first insoluble matter determinator is provided with siphon suction filtering tube, the inlet of described siphon suction filtering tube is arranged on extractor bottom position, guaranteeing that discharge opeing is thorough, described siphonal height is lower than dissolving liquid level;
Described second insoluble matter determinator also includes a sealing member, and described sealing member is provided with agitating device and inlet, and described inlet is connected by pipeline and solvent system;
The leakage fluid dram of the siphon suction filtering tube of the extractor of the second insoluble matter determinator is arranged at the middle and upper part of funnel;
Bottom and the funnel place of the extractor of described second insoluble matter determinator are respectively arranged with heater;
The agitating device of described second insoluble matter determinator is provided with stirring vane, weighing that sample can be carried out as carrier by this stirring vane and reinforced.
2. device according to claim 1, it is characterized in that, described first insoluble matter determinator also includes the first cylinder and condensing tube, described condensing tube and the first cylinder and connects, and lifted by it, the extractor of described condensing tube and the first insoluble matter determinator connects.
3. device according to claim 1, it is characterised in that be additionally provided with drying heater on described steam-return line, be additionally provided with solvent heater outside the solvent compartment of described first insoluble matter determinator.
4. device according to claim 1, it is characterised in that the bottom of described second insoluble matter determinator is connected with the 3rd cylinder.
5. device according to claim 1, it is characterised in that the solvent compartment of described insoluble matter determinator is connected by pipeline and waste collecting device.
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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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| 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 true CN103837423B (en) | 2016-06-15 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN108531206B (en) * | 2018-04-03 | 2020-12-29 | 西南石油大学 | High-evolution pyrobitumen high-temperature circulating dissolving device and method |
| CN109540730B (en) * | 2018-12-19 | 2024-08-20 | 北京英斯派克科技有限公司 | Unmanned environment-friendly insoluble content measuring device and method |
| CN118258713A (en) * | 2022-12-27 | 2024-06-28 | 中国石油天然气股份有限公司 | Insoluble matter measuring system and insoluble matter content measuring method |
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| CN2044255U (en) * | 1988-10-19 | 1989-09-13 | 张虞安 | Purrifying device for bilirubin |
| CN202256009U (en) * | 2011-10-17 | 2012-05-30 | 中国石油化工股份有限公司 | Device for measuring asphaltene in wax oil fraction |
| CN202478644U (en) * | 2011-12-28 | 2012-10-10 | 武汉信嘉和诚药物化学有限公司 | Soxhlet extractor with stirring function |
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| JP3195816B2 (en) * | 1992-01-31 | 2001-08-06 | 日本真空技術株式会社 | Method and apparatus for measuring sample vapor pressure |
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Patent Citations (3)
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|---|---|---|---|---|
| CN2044255U (en) * | 1988-10-19 | 1989-09-13 | 张虞安 | Purrifying device for bilirubin |
| CN202256009U (en) * | 2011-10-17 | 2012-05-30 | 中国石油化工股份有限公司 | Device for measuring asphaltene in wax oil fraction |
| CN202478644U (en) * | 2011-12-28 | 2012-10-10 | 武汉信嘉和诚药物化学有限公司 | Soxhlet extractor with stirring function |
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