CN102607917A - Determination method for high-content quinoline insoluble - Google Patents
Determination method for high-content quinoline insoluble Download PDFInfo
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- CN102607917A CN102607917A CN2012100644847A CN201210064484A CN102607917A CN 102607917 A CN102607917 A CN 102607917A CN 2012100644847 A CN2012100644847 A CN 2012100644847A CN 201210064484 A CN201210064484 A CN 201210064484A CN 102607917 A CN102607917 A CN 102607917A
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Abstract
The invention relates to the technical field of detection asphalt or semicoke quinoline insoluble in laboratories, in particular to a determination method for high-content quinoline insoluble, which includes filter paper mounting, sample quinoline dissolving, sample centrifuging and leaching. The method is characterized in that residue in a centrifuge tube after sample centrifugation is subjected to twice ultrasonic dissolving and twice centrifuging under the condition of heat insulation, and insoluble is washed by more than three types of solvents. Compared with the prior art, the determination method has the advantages that firstly, sample dissolving is operated in an ultrasonic oscillation way, so that dissolving is more complete and detection results can be truer and more accurate; secondly, since the sample is subjected to twice dissolving and twice centrifuging, dissolving of solvend is more complete, and leaching time is shortened; and thirdly, hot water is fed into a leaching funnel spacer bush during leaching to keep the temperature of the sample and quinoline solution within 70-85 DEG C, so that dissolving of solvend is quickened; and in addition, viscosity of leached matters is lowered, and accordingly the washing process can be smoother.
Description
Technical field
The present invention relates to pitch or semicoke quinoline insolubles detection technique field in the laboratory, particularly a kind of assay method of high-load quinoline insolubles.
Background technology
It is a lot of to characterize the index that coal-tar pitch forms, and commonly used have quinoline insolubles, toluene insolubles etc., and the content of quinoline insolubles is very big to the performance impact of adhesive property, carbon yield and the relevant raw material of wood-charcoal material of coal-tar pitch.
Quinoline insolubles (being called for short QI) is the part that is insoluble to toluene and quinoline in the asphalt component, is the inert fraction in the pitch.Quinoline insolubles content in the pitch is one of main factor that forms mutually in the middle of the influence.The content of phase secondary quinoline insolubles commonly used is represented in the middle of the pitch, and what of the middle phase content of pitch are the size of secondary quinoline insolubles content reflected, the detection of the middle phase content of pitch thermal transition product becomes particularly important in production and research.
Low QI content coal tar, bitumen can detect with current national standard GB/T2293-1997 method.But for high-load bitumen, coal-tar pitch carbonizing production (400～490 ℃ of charing products therefroms); It is then relatively more difficult to utilize the act.std method to measure its QI, and there is certain defective in it: detecting used carrier is filter paper, for the higher sample of QI content; Viscosity is bigger; Be prone to cause the filter paper duct to stop up, the solvent wash difficulty, suction filtration speed is extremely slow; In addition, the cooling of hot quinoline is very fast, and dissolving power reduces, and washs not thoroughly, causes detection time long, cause measured value be difficult for parallel, accuracy is low, poor repeatability.
Summary of the invention
The object of the present invention is to provide a kind of assay method of high-load quinoline insolubles; Overcome the deficiency of prior art; Be applicable to the high-load quinoline insolubles that detects in pitch or the semicoke; Alleviate the problem that the filter paper duct is stopped up, solvent wash is difficult, make testing process faster, testing result is more accurate.
For realizing above-mentioned purpose, the present invention adopts following technical scheme to realize:
A kind of assay method of high-load quinoline insolubles; Comprise filter paper, the dissolving of sample quinoline, centrifugal, the suction filtration of sample are installed; Under heat-retaining condition, the residue in the centrifuge tube of the centrifugal back of sample being carried out twice ultrasonic dissolution separates with two times centrifugal; At last insolubles is washed with solvent more than three kinds, its processing procedure specifically comprises the steps:
1) add 20～100ml in the residue in the centrifuge tube of the centrifugal back of sample, temperature is 70～85 ℃ a hot quinoline, adopts the ultrasonic oscillation mode to dissolve, and ultrasonic frequency is 40～60Hz, concussion 10～30min;
2) potpourri in the step 1) centrifuge tube is carried out the centrifuging first time, centrifuge speed is 3000～4500r/min, and centrifugation time is 5～30min, and the dissolved matter in the centrifuge tube removes suction filtration;
3) to step 2) add 20～100ml in the insolubles in the centrifuge tube after centrifugal, temperature is 70～85 ℃ a hot quinoline, adopts the ultrasonic oscillation mode to dissolve, ultrasonic frequency is 40～60Hz, concussion 10～30min;
4) potpourri in the step 3) centrifuge tube is carried out the centrifuging second time, centrifuge speed is 3000～4500r/min, and centrifugation time is 5～30min, and the dissolved matter in the centrifuge tube removes suction filtration;
5) all be transferred to remaining insolubles in the centrifuge tube of the centrifugal back of step 4) on the filter paper; And use the hot quinoline of 30～100ml, 30～100ml toluene, 30～100ml washing with acetone suction filtration successively; In the spacer of suction funnel, feed 75～85 ℃ of hot water during suction filtration continuously; At last, filter paper is dried to constant weight.
Said sample is a quinoline insolubles content greater than 10～70% spun pitch, mesophase pitch and semicoke, and granularity is 0.15～0.20mm.
Said quinoline, toluene, acetone are that analysis is pure.
Compared with prior art, the invention has the beneficial effects as follows:
1) sample dissolution adopts the ultrasonic oscillation mode, dissolves more fully, makes more true and accurate of testing result.
2) sample makes the solvend dissolving more abundant through twice dissolving, secondary centrifuging, has shortened the suction filtration time.
3) in the suction filtration process, in the suction funnel spacer, feed hot water thermal insulating, make the temperature of sample and quinoline solvent remain on 70～85 ℃, quickened the dissolving of sample solvend; In addition, reduced by suction filtration material viscosity, the wetted area on filter paper reduces relatively, has avoided stickum to stop up the filter paper duct simultaneously, makes the process of washing more smooth and easy.
4) accuracy of the inventive method testing result is high, good reproducibility, and parallel appearance error is little.
Embodiment
Describe in further detail below in conjunction with the accompanying drawing specific embodiments of the invention.
Embodiment 1
Sample is for making the spun pitch of charcoal fiber, 240 ℃ of softening points, granularity 0.15mm.Accurately take by weighing sample 0.9000g, sample is put into centrifuge tube, add 80 ℃ of quinoline 20ml dissolvings; Shake 15min in the ultrasonic oscillation device, concussion frequency 40Hz puts into hydro-extractor then; Under 4000r/min; Behind the centrifugal 20min, the clear liquid in the centrifuge tube is slowly poured into suction filtration in the suction funnel that is placed with filter paper, in the suction funnel spacer, fed 80 ℃ of hot water thermal insulatings in the suction filtration process continuously.It is centrifugal once more in centrifuge tube, to add 80 ℃ of quinoline 20ml again, and residue in the centrifuge tube all is transferred on the filter paper, washs suction filtration with hot quinoline 50ml, toluene 80ml, acetone 80ml successively.The parallel appearance of this sample testing result is 31.9%, 32.2%.
Embodiment 2
Sample is a mesophase pitch, and softening point is greater than 300 ℃, granularity 0.15mm.Accurately take by weighing sample 0.8000g, sample is put into centrifuge tube, add 80 ℃ of quinoline 20ml dissolvings; Shake 15min in the ultrasonic oscillation device, concussion frequency 40Hz puts into hydro-extractor then; Under 3500r/min; Behind the centrifugal 20min, the clear liquid in the centrifuge tube is slowly poured into suction filtration in the suction funnel that is placed with filter paper, in the suction funnel spacer, fed 80 ℃ of hot water thermal insulatings in the suction filtration process continuously.It is centrifugal once more in centrifuge tube, to add 80 ℃ of quinoline 20ml again, and residue in the centrifuge tube all is transferred on the filter paper, washs suction filtration with hot quinoline 50ml, toluene 80ml, acetone 50ml successively.Test parallel appearance result and be respectively 48.9%, 49.2%.
Embodiment 3
Sample is semicoke (480 ℃ of charing intermediate products of pitch), granularity 0.15mm.Accurately take by weighing sample 1.000g, sample is put into centrifuge tube, add 80 ℃ of quinoline 20ml dissolvings; Shake 15min in the ultrasonic oscillation device, concussion frequency 50Hz puts into hydro-extractor then; Under 3500r/min; Behind the centrifugal 20min, slowly poured into suction filtration in the suction funnel that is placed with filter paper the stillness of night in the centrifuge tube, in the suction funnel spacer, feed 80 ℃ of hot water thermal insulatings in the suction filtration process continuously.It is centrifugal once more in centrifuge tube, to add 80 ℃ of quinoline 20ml again, and residue in the centrifuge tube all is transferred on the filter paper, washs suction filtration with hot quinoline 50ml, toluene 50ml, acetone 50ml successively.Test parallel appearance result and be respectively 72.4%, 72.9%.
Claims (3)
1. the assay method of a high-load quinoline insolubles; Comprise filter paper, the dissolving of sample quinoline, centrifugal, the suction filtration of sample are installed; It is characterized in that; Under heat-retaining condition, the residue in the centrifuge tube of the centrifugal back of sample is carried out twice ultrasonic dissolution and separate with two times centrifugal, at last insolubles is washed with solvent more than three kinds, its processing procedure specifically comprises the steps:
1) add 20～100ml in the residue in the centrifuge tube of the centrifugal back of sample, temperature is 70～85 ℃ a hot quinoline, adopts the ultrasonic oscillation mode to dissolve, and ultrasonic frequency is 40～60Hz, concussion 10～30min;
2) potpourri in the step 1) centrifuge tube is carried out the centrifuging first time, centrifuge speed is 3000～4500r/min, and centrifugation time is 5～30min, and the dissolved matter in the centrifuge tube removes suction filtration;
3) to step 2) add 20～100ml in the insolubles in the centrifuge tube after centrifugal, temperature is 70～85 ℃ a hot quinoline, adopts the ultrasonic oscillation mode to dissolve, ultrasonic frequency is 40～60Hz, concussion 10～30min;
4) potpourri in the step 3) centrifuge tube is carried out the centrifuging second time, centrifuge speed is 3000～4500r/min, and centrifugation time is 5～30min, and the dissolved matter in the centrifuge tube removes suction filtration;
5) all be transferred to remaining insolubles in the centrifuge tube of the centrifugal back of step 4) on the filter paper; And use the hot quinoline of 30～100ml, 30～100ml toluene, 30～100ml washing with acetone suction filtration successively; In the spacer of suction funnel, feed 75～85 ℃ of hot water during suction filtration continuously; At last, filter paper is dried to constant weight.
2. the assay method of a kind of high-load quinoline insolubles according to claim 1 is characterized in that, said sample is a quinoline insolubles content greater than 10～70% spun pitch, mesophase pitch and semicoke, and granularity is 0.15～0.20mm.
3. the assay method of a kind of high-load quinoline insolubles according to claim 1 is characterized in that, said quinoline, toluene, acetone are that analysis is pure.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103028581A (en) * | 2011-09-29 | 2013-04-10 | 上海宝钢化工有限公司 | Handling method of sand core crucible used for detecting insoluble quinoline |
| CN103048212A (en) * | 2012-11-09 | 2013-04-17 | 红塔烟草(集团)有限责任公司 | Determining method of hot-water soluble matters of papermaking-method reproduced tobaccos |
| CN103823023A (en) * | 2014-02-27 | 2014-05-28 | 北京英斯派克科技有限公司 | Apparatus for determining insoluble substance |
| CN103837692A (en) * | 2014-02-27 | 2014-06-04 | 北京英斯派克科技有限公司 | Quinoline insoluble matter measuring device |
| CN104297107A (en) * | 2013-07-15 | 2015-01-21 | 上海宝钢化工有限公司 | Shape and particle size measuring method for tar residue |
| CN107884304A (en) * | 2017-11-24 | 2018-04-06 | 神华集团有限责任公司 | The assay method of tetrahydrofuran DDGS in coal liquefaction residue |
| CN109355096A (en) * | 2018-12-15 | 2019-02-19 | 陕西延长石油（集团）有限责任公司 | A kind of method that coal-derived oils are separated by solid-liquid separation |
| CN110567852A (en) * | 2019-10-17 | 2019-12-13 | 北京旭阳科技有限公司 | Rapid detection method for quinoline insoluble substances in asphalt |
| CN111006962A (en) * | 2019-12-30 | 2020-04-14 | 陕西延长石油（集团）有限责任公司 | Method for rapidly determining content of toluene insoluble substances in heavy oil |
| CN112577848A (en) * | 2020-11-24 | 2021-03-30 | 本钢板材股份有限公司 | Method for determining quinoline insoluble substances in coal tar pitch |
| CN112834382A (en) * | 2021-04-06 | 2021-05-25 | 枣庄杰富意振兴化工有限公司 | Method for detecting content of quinoline insoluble substances |
| CN113740271A (en) * | 2020-05-28 | 2021-12-03 | 北京旭阳科技有限公司 | Detection method of quinoline insoluble substance |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058984A (en) * | 1991-06-04 | 1992-02-26 | 华东冶金学院 | The method of separating quinoline non-soluble composition in the coal tar |
| CN1208854A (en) * | 1997-08-14 | 1999-02-24 | 杨素习 | Method for determining contents of precipitate in crude oil |
| JP2004109090A (en) * | 2002-09-20 | 2004-04-08 | Cosmo Oil Co Ltd | Analysis method of asphalt |
| CN101294090A (en) * | 2007-04-25 | 2008-10-29 | 淄博矿业集团有限责任公司 | Fine purification method for coal tar pitch |
| CN102095615A (en) * | 2009-12-11 | 2011-06-15 | 武侯区巅峰机电科技研发中心 | Method for determining contents of asphaltine, colloid and wax |
-
2012
- 2012-03-12 CN CN201210064484.7A patent/CN102607917B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058984A (en) * | 1991-06-04 | 1992-02-26 | 华东冶金学院 | The method of separating quinoline non-soluble composition in the coal tar |
| CN1208854A (en) * | 1997-08-14 | 1999-02-24 | 杨素习 | Method for determining contents of precipitate in crude oil |
| JP2004109090A (en) * | 2002-09-20 | 2004-04-08 | Cosmo Oil Co Ltd | Analysis method of asphalt |
| CN101294090A (en) * | 2007-04-25 | 2008-10-29 | 淄博矿业集团有限责任公司 | Fine purification method for coal tar pitch |
| CN102095615A (en) * | 2009-12-11 | 2011-06-15 | 武侯区巅峰机电科技研发中心 | Method for determining contents of asphaltine, colloid and wax |
Non-Patent Citations (3)
| Title |
|---|
| 孙培山 等: "降低煤焦油中灰分和喹啉不溶物的研究", 《煤化工》, 31 December 2011 (2011-12-31) * |
| 王秀丹 等: "热溶过滤法脱除煤焦油沥青中喹啉不溶物的研究", 《炭素技术》, vol. 26, no. 1, 31 December 2007 (2007-12-31) * |
| 赵永红 等: "《中华人民共和国国家标准 GB/T2293-2008》", 13 May 2008, article "焦化沥青类产品喹啉不溶物试验方法" * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103028581B (en) * | 2011-09-29 | 2014-10-22 | 上海宝钢化工有限公司 | Handling method of sand core crucible used for detecting insoluble quinoline |
| CN103028581A (en) * | 2011-09-29 | 2013-04-10 | 上海宝钢化工有限公司 | Handling method of sand core crucible used for detecting insoluble quinoline |
| CN103048212A (en) * | 2012-11-09 | 2013-04-17 | 红塔烟草(集团)有限责任公司 | Determining method of hot-water soluble matters of papermaking-method reproduced tobaccos |
| CN104297107A (en) * | 2013-07-15 | 2015-01-21 | 上海宝钢化工有限公司 | Shape and particle size measuring method for tar residue |
| CN103837692B (en) * | 2014-02-27 | 2016-03-02 | 北京英斯派克科技有限公司 | A kind of quinoline non-soluble object measuring device |
| CN103837692A (en) * | 2014-02-27 | 2014-06-04 | 北京英斯派克科技有限公司 | Quinoline insoluble matter measuring device |
| CN103823023A (en) * | 2014-02-27 | 2014-05-28 | 北京英斯派克科技有限公司 | Apparatus for determining insoluble substance |
| CN107884304A (en) * | 2017-11-24 | 2018-04-06 | 神华集团有限责任公司 | The assay method of tetrahydrofuran DDGS in coal liquefaction residue |
| CN109355096A (en) * | 2018-12-15 | 2019-02-19 | 陕西延长石油（集团）有限责任公司 | A kind of method that coal-derived oils are separated by solid-liquid separation |
| CN110567852A (en) * | 2019-10-17 | 2019-12-13 | 北京旭阳科技有限公司 | Rapid detection method for quinoline insoluble substances in asphalt |
| CN111006962A (en) * | 2019-12-30 | 2020-04-14 | 陕西延长石油（集团）有限责任公司 | Method for rapidly determining content of toluene insoluble substances in heavy oil |
| CN113740271A (en) * | 2020-05-28 | 2021-12-03 | 北京旭阳科技有限公司 | Detection method of quinoline insoluble substance |
| CN112577848A (en) * | 2020-11-24 | 2021-03-30 | 本钢板材股份有限公司 | Method for determining quinoline insoluble substances in coal tar pitch |
| CN112834382A (en) * | 2021-04-06 | 2021-05-25 | 枣庄杰富意振兴化工有限公司 | Method for detecting content of quinoline insoluble substances |
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