CN103837692B - A kind of quinoline non-soluble object measuring device - Google Patents
A kind of quinoline non-soluble object measuring device Download PDFInfo
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- CN103837692B CN103837692B CN201410069740.0A CN201410069740A CN103837692B CN 103837692 B CN103837692 B CN 103837692B CN 201410069740 A CN201410069740 A CN 201410069740A CN 103837692 B CN103837692 B CN 103837692B
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Abstract
The invention discloses a kind of determinator of insolubles, comprise extracting barrel, funnel and beaker, described extracting barrel is positioned at the top of funnel, and described funnel is connected with beaker; Be provided with seal above described extracting barrel, described seal is provided with inlet, described inlet is connected with liquid-adding device; Described seal is also provided with stirring apparatus, and described stirring apparatus is connected with air motor; Described device also comprises upper cylinder, and described upper cylinder is connected with seal; Described device also comprises lower cylinder, and described lower cylinder is connected with bottom of device.The present invention can meet the requirement that quinoline insolubles measures, and concentrates and achieve liquid feeding, heating, stirring and filtration experiment process, and simple and reliable for structure, requires greatly to reduce to operating personnel; And substantially reduce experimental period, improve work efficiency, avoid operating personnel's Long contact time chemical reagent simultaneously, ensure that personal security.
Description
Technical field
The invention belongs to instrumental analysis field, be specifically related to a kind of quinoline non-soluble object measuring device.
Background technology
The potpourri that coal tar is made up of chemical compound lot, its principal ingredient is applicable to produce needle coke completely, but wherein containing more quinoline insolubles, therefore directly can not produce needle coke with the pitch that coal tar processing obtains.Quinoline insolubles is called for short QI, its average molecular mass is that 1800 ~ 2600, C/H atomic ratio is greater than 1.67, can be divided into a primary QI of QI(by the formation of QI) and the secondary QI of secondary QI(), primary QI exists in coal tar, and during coal tar distillation, it is transferred in pitch.And the aromatic polymer that the molecular weight that secondary QI is pitch to be formed in heating process is larger, be present in pitch with the form of solids.
Quinoline insolubles (QI) is conducive to the physical strength and the electric conductivity that improve carbon product, has certain restriction to the expansion in carbon product roasting.But QI is too high, the mobility of pitch can be made to reduce, be unfavorable for the processing of later stage carbon product.
In the experimentation that current quinoline insolubles measures; often can carry out dissolution filter experiment to measured matter; the assay method of current quinoline insolubles utilizes pure manually operated method to test; in experimentation, need operating personnel's long-time operation to complete; the waste and the work efficiency that so not only cause resource are low; the most important thing is to allow operating personnel's Long contact time toxic gas, very large harm is caused to the health of human body of operating personnel.
Summary of the invention
There are the first-class problems of safety for measuring quinoline insolubles at present, the invention provides a kind of device that can measure quinoline insolubles, achieve harmful gas in quinoline insolubles mensuration process completely isolated, and the arrangement achieves liquid feeding, heating, stirring, filtration all realize automation mechanized operation.
Experimental provision of the present invention comprises extracting barrel, funnel and beaker, and described extracting barrel is positioned at the top of funnel, and described funnel is connected with beaker; Be provided with seal above described extracting barrel, described seal is provided with inlet, described inlet is connected with liquid-adding device; Described seal is also provided with stirring apparatus; Described stirring apparatus is connected with air motor, and described air motor can provide power source for stirring apparatus, by using throttling valve and pressure regulator valve, can realize the adjustment of torsion when stirring and rotating speed.The class formation that described extracting barrel is well known to those skilled in the art, such as Soxhlet extractor, comprises steam rise pipeline and a U trap, and can configure the structures such as condenser pipe, and extracting barrel of the present invention does not comprise steam rise pipeline.
Described device also comprises upper cylinder, described upper cylinder is connected with seal, lifting and the decline of whole stirring apparatus and packoff can be realized, filtration paper cylinder can be put into when promoting or load onto stirring vane, the inner sealing of extracting barrel can be realized after decline, reduce harmful gas and externally volatilize.
Described device also comprises lower cylinder, and described lower cylinder is connected with the bottom of device (such as lower cylinder is connected with the base being placed with beaker and funnel), can realize lifting and the decline of funnel.By lower cylinder drive funnel decline after, funnel can be taken out and filtration paper cylinder is put into, cylinder drive funnel rise after can with enhancing tube bottom dock, formed confined space.
Preferably, opening sealing place of described device arranges viton seal ring sealing.
Preferably, described device also comprises solution preheating device, and described solution preheating device is positioned on the pipeline between inlet and liquid-adding device.In one embodiment of the invention, described solution preheating device is tube heater, solution preheating device adopts pipeline heating mode, adopts SUS316 material to be pipe material, avoids solution and corrosive pipeline, external heating adopts cast aluminium heating, pipeline is cast directly in cast aluminum heaters inside, the maximized increase hot face of energy, improves the speed of heating like this, temperature controls to adopt closed-loop control system, and control temperature accuracy can reach ± and 0.1 degree.
Preferably, described device also comprises middle part well heater, and described middle part well heater is positioned on steam rise pipeline.In the middle part of this, the effect of well heater is for providing constant thermal source when doing quinoline insolubles experiment, the burnt grain of accelerate dissolution.In one embodiment of the invention, middle part well heater adopts cast aluminum heaters mode, uses two semicircular clamping structure, can firmly contact with heated object.
Preferably, described device also comprises bottom heater, and described bottom heater can be beaker heat supply.In an embodiment of the present invention, bottom heater adopts cast aluminum heaters mode.After filtration completes, well heater can be utilized to carry out drying and processing in advance to filtration filter paper, reduce the diffusion of harmful gas in outside.
Preferably, described liquid-adding device comprises some peristaltic pumps.Carry out liquid feeding by peristaltic pump, can realize automatic liquid-feeding at any time, accuracy can reach ± 0.01ml.
Preferably, extracting the condenser that cylinder connects is spherical condensation tube, increases the external diameter of its condenser pipe and the surface area of interior ball, its condensation effect can be made better.
Preferably, described device also comprises valve means and vacuum plant; Described device is arranged in can, and described valve means is arranged on can.Described vacuum plant is used for the discharge of harmful gas in can.Described can adopt stainless steel welded forming, and weld seam carries out full weld welding technology, and has carried out performing leak test after part machine-shaping.Described valve means can carry out return-air when vacuumizing gas-tight silo, and this valve means can adopt not only high temperature resistant but also corrosion resistant solenoid valve.
The present invention utilizes the lifting of cylinder and declines and realizes putting filter paper and opening sealing, and opening sealing place adopts viton seal ring sealing, prevents the diffusion of toxic gas in experimentation, ensure that the health of human body of operating personnel.The present invention adds input duct at top seal parts place, can be implemented in the function of liquid feeding at any time in experimentation.The stirring action utilizing air motor to drive stirring vane to carry out in experimentation.Installed heater element additional in extracting barrel outside, for do quinoline experiment in thermal source is provided.The present invention all adopts gas-powered in control, avoids the generation of electrostatic, plays explosion-proof.The present invention adopts external electromagnetic valve to control, and can realize Automated condtrol.
This instrument is applicable to the test detecting quinoline insolubles in coal-tar pitch, modified pitch, coal asphalt oil for building up highway, wood preserving oil and carbon black coking raw material oil.The invention solves the mensuration meeting quinoline insolubles with a kind of constructional device, and the harmful gas in quinoline insolubles mensuration process is completely isolated, and with the addition of the pre-heating system of solution on this basis, liquid feeding, heating, stirring, filtration all realize automation mechanized operation, what whole experimentation was become is easy and simple to handle, and experiment needed raw material only need press start key after getting all the ready.Device of the present invention can adopt programmable controller PLC to control, and realizes whole automation of motions, and the function that can realize mainly comprises: process, the vacuum such as pre-heating system, liquid feeding, heating, stirring, filtration of solution.
The present invention can achieve liquid feeding, heating, stirring and filtration experiment process, and simple and reliable for structure, requires greatly to reduce to operating personnel; And substantially reduce experimental period, improve work efficiency, avoid operating personnel's Long contact time chemical reagent simultaneously, ensure that personal security.
Accompanying drawing explanation
The structural representation of Fig. 1, quinoline non-soluble object measuring device.
The illustrative view of functional configuration of Fig. 2, insolubles determinator.
Fig. 3, quinoline non-soluble object measuring device off working state schematic diagram.
Accompanying drawing identifies:
1, condenser pipe; 2, extracting barrel; 3, funnel; 4, O type circle; 5, beaker; 6, stirring vane; 7, inlet; 8, air motor; 9, upper cylinder; 10, lower cylinder; 11, tube heater; 12, middle part well heater; 13, bottom heater; 14, the first peristaltic pump; 15, the second peristaltic pump; 16, the 3rd peristaltic pump; 17, can; 18, O-ring seal; 19, filtration paper cylinder; 20, Jiao Li; 21, seal.
Embodiment
Be below a preferred embodiment of the present invention, it is only used as the explanation of the application instead of restriction.
See Fig. 1, experimental provision of the present invention comprises extracting barrel 2, funnel 3 and beaker 5, and described extracting barrel 2 is positioned at the top of funnel 3, and described funnel 3 is connected with beaker 5; Be provided with seal 21 above described extracting barrel 2, described seal 21 is provided with inlet 7 and stirring apparatus, and described stirring apparatus comprises stirring vane 6, and described inlet 7 is connected with liquid-adding device.This device also comprises upper cylinder 9, lower cylinder 10 and air motor 8, and comprises solution preheating device, middle part well heater 12 and bottom heater 13.
Wherein, described stirring apparatus is connected with air motor 8, and described air motor 8 can provide power source for stirring apparatus, by using throttling valve and pressure regulator valve, and the torsion of stirring vane 6 and the adjustment of rotating speed when can realize stirring.
Described upper cylinder 9 is connected with seal 21, can realize lifting and the decline of whole stirring apparatus and packoff, can load onto stirring vane 6, can realize the inner sealing of extracting barrel 2 after decline when promoting, and reduces harmful gas and externally volatilizees.Described lower cylinder 10 is connected with the base being placed with beaker 5 and funnel 3, can realize lifting and the decline of funnel 3 and beaker 5.Lower cylinder 10 drive funnel 3 decline after, funnel 3 can be taken out and filtration paper cylinder 19 (see Fig. 3) is put into, cylinder drive funnel 3 rise after can with enhancing tube bottom dock, formed confined space.
In this device, sealing place of seal opening can adopt viton seal ring 18 or O shape circle 4 to seal it, to avoid release of toxic gas.
Described solution preheating device is tube heater 11, solution preheating device adopts pipeline heating mode, SUS316 material is adopted to be pipe material, avoid solution and corrosive pipeline, external heating adopts cast aluminium heating, pipeline is cast directly in cast aluminum heaters inside, the maximized increase hot face of such energy, improve the speed of heating, temperature controls to adopt closed-loop control system, and control temperature accuracy can reach ± and 0.1 degree.
Described middle part well heater 12 is positioned on steam rise pipeline.In the middle part of this, the effect of well heater 12 is for providing constant thermal source when doing quinoline insolubles experiment, the burnt grain of accelerate dissolution.Middle part well heater 12 can adopt cast aluminum heaters mode, uses two semicircular clamping structure, can firmly contact with heated object.
Described bottom heater 13 can be beaker heat supply.Bottom heater 13 can be cast aluminum heaters in an embodiment of the present invention.After filtration completes, well heater can be utilized to carry out drying and processing in advance to filtration filter paper 19, reduce the diffusion of harmful gas in outside.
Described liquid-adding device is peristaltic pump system.Carry out liquid feeding by peristaltic pump, can realize automatic liquid-feeding at any time, accuracy can reach ± 0.01ml.Liquid-adding device shown in Fig. 1 comprises the first peristaltic pump 14, second peristaltic pump 15 and the 3rd peristaltic pump 16, and those skilled in the art also can increase and decrease it as required.
Described device also comprises can 17 and a vacuum plant.Described vacuum plant is used for the discharge of harmful gas in can 17.Described can 17 can adopt stainless steel welded forming, and weld seam carries out full weld welding technology, and has carried out performing leak test after part machine-shaping.
In this device, condenser 1 adopts spherical condensation tube, increases the external diameter of its condenser pipe and the surface area of interior ball, makes its condensation effect better.
See Fig. 2, this device can also comprise a main control unit, and include the actuating unit of air motor, upper cylinder and bottomed cylinder, vacuum pump, comprise the liquid-adding device of the first peristaltic pump 14, second peristaltic pump 15 and the 3rd peristaltic pump 16, valve means and the heating arrangement comprising tube heater 11, bottom heater 13 and middle part well heater 12 controlled by heating controller.Said apparatus is all direct or indirectly controlled by main control unit.Main control unit herein can be programmable controller PLC, also can change to Non-follow control as required.
This device utilizes the lifting of cylinder and declines and realizes putting filter paper and opening sealing, prevents the diffusion of toxic gas in experimentation, ensure that the health of human body of operating personnel.In upper seal 21, place adds inlet 7, can be implemented in the function of liquid feeding at any time in experimentation.The stirring action utilizing air motor to drive stirring vane 6 to carry out in experimentation.Installed heater element additional in extracting barrel 2 outside, for do quinoline experiment in thermal source is provided.The present invention all adopts gas-powered in control, avoids the generation of electrostatic, plays explosion-proof.Adopt external electromagnetic valve to control, can Automated condtrol be realized.
See Fig. 3, when quinoline determination experiment, burnt grain can directly weigh on stirring vane, can reduce the loss that raw material causes in transfer process like this, avoid the error that this link causes result of calculation.
In said apparatus, well heater can increase and decrease as required, and peristaltic pump also can increase as required flexibly.
The present invention can achieve liquid feeding, heating, stirring and filtration experiment process, and simple and reliable for structure, requires greatly to reduce to operating personnel; Substantially reduce experimental period, improve work efficiency, avoid operating personnel's Long contact time chemical reagent simultaneously, ensure that personal security.
Claims (4)
1. an insolubles determinator, comprises extracting barrel, funnel and beaker, it is characterized in that, described extracting barrel is positioned at the top of funnel, and described funnel is connected with beaker; Be provided with seal above described extracting barrel, described seal is provided with inlet, described inlet is connected with liquid-adding device; Described seal is also provided with stirring apparatus, and described stirring apparatus is connected with air motor;
Described insolubles determinator also comprises upper cylinder, and described upper cylinder is connected with seal;
Described insolubles determinator also comprises lower cylinder, and described lower cylinder is connected with bottom insolubles determinator;
Described insolubles determinator also comprises middle part well heater, and described middle part well heater is positioned on steam rise pipeline;
Described insolubles determinator also comprises bottom heater, and described bottom heater can be beaker heat supply.
2. insolubles determinator according to claim 1, is characterized in that, described device also comprises solution preheating device, and described solution preheating device is positioned on the pipeline between inlet and liquid-adding device.
3. insolubles determinator according to claim 1, is characterized in that, described liquid-adding device comprises some peristaltic pumps.
4. insolubles determinator according to claim 1, is characterized in that, described insolubles determinator also comprises valve means and vacuum plant; Described insolubles determinator is arranged in can, and described valve means is arranged on can.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410069740.0A CN103837692B (en) | 2014-02-27 | 2014-02-27 | A kind of quinoline non-soluble object measuring device |
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| CN201410069740.0A CN103837692B (en) | 2014-02-27 | 2014-02-27 | A kind of quinoline non-soluble object measuring device |
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| CN103837692B true CN103837692B (en) | 2016-03-02 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102607917A (en) * | 2012-03-12 | 2012-07-25 | 中钢集团鞍山热能研究院有限公司 | Determination method for high-content quinoline insoluble |
| CN102621029A (en) * | 2012-03-21 | 2012-08-01 | 云南昆钢煤焦化有限公司 | Measurement method of soft asphalt quinoline insoluble substance |
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2014
- 2014-02-27 CN CN201410069740.0A patent/CN103837692B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102607917A (en) * | 2012-03-12 | 2012-07-25 | 中钢集团鞍山热能研究院有限公司 | Determination method for high-content quinoline insoluble |
| CN102621029A (en) * | 2012-03-21 | 2012-08-01 | 云南昆钢煤焦化有限公司 | Measurement method of soft asphalt quinoline insoluble substance |
Non-Patent Citations (7)
| Title |
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| 出口煤焦油喹啉不溶物的测定;牟明仁等;《石油化工高等学校学报》;19970630;第10卷(第2期);32-34 * |
| 对煤沥青中喹啉不溶物分析方法的改进;莫菊青等;《煤化工》;20040831(第113期);45-46,52 * |
| 提高喹啉不溶物测定的准确性;毛艾萍等;《燃料与化工》;20130531;第44卷(第3期);64-65,67 * |
| 测定低含量喹啉不溶物的试验方法;田立等;《炭素技术》;20031231(第125期);10-14 * |
| 焦化沥青类产品喹啉不溶物实验方法;中华人民共和国国家质量监督检验检疫总局等;《中华人民共和国国家标准GB/T2293-2008》;20080513;1-3 * |
| 焦油和沥青中喹啉不溶物的测定;G.R.Romovacek;《炭素技术》;19861231(第5期);13,31-32 * |
| 煤沥青喹啉不溶物及其测定方法稳定性的研究;周顺民等;《炭素技术》;20021231(第118期);12-18 * |
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