CN105238428A - Medium temperature coal pitch modification method and product - Google Patents
Medium temperature coal pitch modification method and product Download PDFInfo
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- CN105238428A CN105238428A CN201510652855.7A CN201510652855A CN105238428A CN 105238428 A CN105238428 A CN 105238428A CN 201510652855 A CN201510652855 A CN 201510652855A CN 105238428 A CN105238428 A CN 105238428A
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Abstract
A medium temperature coal pitch modification method includes the following steps: (1) mixing anhydrous AlCl3 and medium temperature coal pitch which is crushed to the particle size of 0.1 mm or less according to the weight ratio of (2-12):100 in a V-shaped mixer, and then sending into a reaction kettle; (2) introducing N2 to exclude air in the reaction kettle, heating up to 100 DEG C, carrying out heat preservation for 25-35 min, then heating up to 200-320 DEG C, carrying out a reaction for 1-5 h, cooling, and then taking out; and (3) crushing the material obtained after reaction in the step (2), then washing with dilute hydrochloric acid, filtering, carrying out vacuum drying, removing the modifier AlCl3, and thus obtaining the modified medium temperature coal pitch. Compared with raw material pitch, the modified medium temperature coal pitch obtained from modification by the method has higher softening point and coking value, and especially has the QI and beta resin greatly improved; and with the modified medium temperature coal pitch as a binder, a carbon material with excellent structure and properties can be prepared.
Description
Technical field
The present invention relates to method of modifying and the product scope of medium temperature coal pitch.
Background technology
Current comparative maturity and industrially widely used transformation of the way asphalt production technology be thermopolymerization technology and gilsonite vacuum flashing technology, these two kinds of technology can improve the performance of coal-tar pitch to a certain extent, but improve limitation.The Main way that chemical active agent is the research of current coal tar pitch modification is added in coal-tar pitch, use chemical active agent modified coal pitch, not only can promote that coal-tar pitch molecule is cross-linked with each other, improve the molecular-weight average of coal-tar pitch, the volatilization of light constituent in carbonization process can also be stoped, improve the carbon yield of coal-tar pitch.
The people such as B.Grzyb adopt polyacrylonitrile and polyvinylpyridine to carry out modification to coal-tar pitch respectively, research shows, this improves the charing behavior of coal-tar pitch to a great extent, improve the carbon yield (B.Grzyb of coal-tar pitch, J.Machnikowsiki, J.V.Weber, etal.Mechanismofco-pyrolysisofpitchwithpolyvinylpyridine [J] .JournalofAnalyticalandAppliedPyrolysis, 2004,72:121-130.).The people such as B.Petrova use strong oxidizer H
2sO
4, HNO
3, H
2o
2process coal-tar pitch, result shows, in the coal-tar pitch processed, TI and QI content increases, the softening temperature of coal-tar pitch and C/H atomic ratio are improved (Bpetrova, TBudinova, NPetrov, eta1.Effectofdifferentoxidationtreatmentsonthechemicalst ructureandpropertiesofcommercialcoaltarpitch [J] .Carbon, 2005,43:26l-267.).The people such as Song Shihua adopt Vinylstyrene (DVB) and p-tolyl aldehyde (PMB) to carry out modification to coal-tar pitch under the effect of tosic acid, the active small molecular in coal-tar pitch is made to be cross-linked with each other into macromole, effectively can improve the softening temperature of coal-tar pitch, carbon yield, and improve the graphitization characteristic (Song Shihua of coal-tar pitch carbonizing production, Wei Jianning. mechanism of modification research [J] of p-tolyl aldehyde modified coal pitch. Jiujiang journal, 2007 (3): 82-84.).The people such as Zhang Wenjuan adopt phenylacrolein as properties-correcting agent, under the effect of tosic acid, the comparative study of modification is carried out to coal-tar pitch, obtain compared with high fixing carbon and easy graphited modified coal pitch (WenjuanZhang, TiehuLi, MengLu, etal.Acomparativestudyofcharacteristicsandcarbonizationb ehaviorsofthreemodifiedcoaltarpitches [J] .Carbon, 2013,60:564.).The people such as Xiao Jing adopts by adding oleic acid or dibutyl phthalate is not more than 40 μm of powdered carbons as properties-correcting agent with superfine graphite powder or granularity in molten asphalt, reach under the prerequisite guaranteeing asphalt high-temperature coking value, improve the object (CN101812235A) of the rheological of pitch under kneading temperature (160 ~ 180 DEG C).The people such as Ren Lihua adopt formaldehyde, trioxymethylene or paraformaldehyde to carry out modification as the coal-tar pitch of properties-correcting agent to softening temperature < 130 DEG C, by controlling the temperature of polyreaction, pressure and time, produce softening temperature adjustable within the specific limits, softening range is wide, plasticity-is large, has the modified coal pitch (CN1760331A) of linear resin molecular structure.People's N-Methyl pyrrolidone such as Cukier and coal tar fraction make properties-correcting agent, the regulation and control to pitch Group Component are realized by physical method, prepare QI component concentration and median size low, ash content is lower, TI component and the high modified pitch (US4604184) of resin content.But the properties-correcting agent that aforesaid method uses costly, or modified technique is complicated, is difficult to industrial applications.
Summary of the invention
The technical problem to be solved in the present invention is, overcome the above-mentioned defect that prior art exists, a kind of medium temperature coal pitch method of modifying is provided, this method of modifying operation steps is simple, the properties-correcting agent low price used, medium temperature coal pitch softening temperature, coking value can be effectively improved, and more Effective Regulation can be carried out to coal-tar pitch microtexture.
The present invention is the technical scheme solving the employing of its technical problem: a kind of medium temperature coal pitch method of modifying, comprises the following steps:
(1) raw material mixing: by anhydrous AlCl
3mix in mixer by weight 2 ~ 12wt% with medium temperature coal pitch, the time of mixing is 40-80min;
(2) react: step (1) gained mixing raw material is sent in reactor, passes into N
2get rid of the air in reactor, first temperature is risen to 95-105 DEG C, preferred 98-102 DEG C, and be incubated 25-35min, preferred 30-35min, then, then be warming up to 200 ~ 320 DEG C, reaction 1 ~ 5h, is cooled to room temperature;
(3) wash: by cooling gained crushing material after step (2) reaction, then use 0.08-0.12mol/L, the dilute hydrochloric acid washing of preferred 0.1mol/L, filter more than 2 times, vacuum-drying is to remove modifier A lCl
3and moisture, obtain modified medium temperature coal pitch.
Preferably, in step (1), described anhydrous AlCl
3purity be more than 98%.Described anhydrous AlCl
3with medium temperature coal pitch by weight preferable range be 4 ~ 10wt%, be more preferably 6 ~ 8wt%.The time of described mixing can be 50-70min.
Preferably, in step (2), described in the N that passes into
2flow is the air that 200ml/min gets rid of in reactor.The described temperature rise rate heated up again is 5-10 DEG C/min; Preferred temperature rise rate is 4-6 DEG C/min.The temperature of described reaction is preferably 220 DEG C-300 DEG C, and soaking time is 2 ~ 5h.
Preferably, in step (3), number of times >=3 time of described washing.
Use the modification medium temperature coal pitch that the inventive method obtains, softening temperature is 98.6 ~ 152.2 DEG C; Coking value is 53.5 ~ 64.0%; Described race component: quinoline insolubles QI content is 5.73% ~ 17.20%; Toluene insolubles BI content is 20.02% ~ 45.17%, β resin TI-QS content is 15.66 ~ 26.24%.
The present invention adopts anhydrous AlCl
3carry out modification as properties-correcting agent to medium temperature coal pitch, technique is simple, and effectively can improve softening temperature and the coking value of medium temperature coal pitch, the more important thing is, the method can increase substantially β resin content, the microscopic optical structure of Effective Regulation coal-tar pitch charcoal.
Accompanying drawing explanation
The modified coal pitch microscopic optical structure through 420 DEG C carbonization 60min after of accompanying drawing 1 prepared by embodiment 1.
The modified coal pitch microscopic optical structure through 420 DEG C carbonization 60min after of accompanying drawing 2 prepared by embodiment 2.
The modified coal pitch microscopic optical structure through 420 DEG C carbonization 60min after of accompanying drawing 3 prepared by embodiment 3.
The modified coal pitch microscopic optical structure through 420 DEG C carbonization 60min after of accompanying drawing 4 prepared by embodiment 4.
The modified coal pitch microscopic optical structure through 420 DEG C carbonization 60min after of accompanying drawing 5 prepared by embodiment 5.
The modified coal pitch microscopic optical structure through 420 DEG C carbonization 60min after of accompanying drawing 6 prepared by embodiment 6.
The metaloscope that the microscopic optical structure of each embodiment is Lab.A1 by model above records.
Embodiment
In following all embodiments: anhydrous AlCl used
3purity more than 98%, modifying process passes into the N that flow is 200ml/min
2protect, no longer describe in following specific examples.
Embodiment 1: by anhydrous AlCl
3be crushed to particle diameter be below 0.1mm medium temperature coal pitch by weight 6wt%, in V-Mixer, mix 60min after send in reactor; Freely be warming up to 100 DEG C and be incubated half an hour, then 220 DEG C are warmed up to 5 DEG C/min temperature rise rate, and be incubated 3h, after cooling, modified coal-tar pitch is taken out, and be obtained modified coal pitch to remove properties-correcting agent 3 times with the salt acid elution that concentration is 0.1mol/L.Accompanying drawing 1 is the microscopic optical structure of prepared modified coal pitch after 420 DEG C of carbonization 60min.
Embodiment 2
By anhydrous AlCl
3be crushed to particle diameter be below 0.1mm medium temperature coal pitch by weight 6wt%, in V-Mixer, mix 1h after send in reactor; Freely be warming up to 100 DEG C and be incubated half an hour, then 260 DEG C are warmed up to 5 DEG C/min temperature rise rate, and be incubated 3h, after cooling, modified coal-tar pitch is taken out, and be obtained modified coal pitch to remove properties-correcting agent 3 times with the salt acid elution of concentration 0.1mol/L.Accompanying drawing 2 is for being the microscopic optical structure of prepared modified coal pitch in crucible electrical resistance furnace after 420 DEG C of carbonization 60min.
Embodiment 3
By anhydrous AlCl
3be crushed to particle diameter be below 0.1mm medium temperature coal pitch by weight 6wt%, in V-Mixer, mix 1h after send in reactor; Freely be warming up to 100 DEG C and be incubated half an hour, then 300 DEG C are warmed up to 5 DEG C/min temperature rise rate, and be incubated 3h, after cooling, modified coal-tar pitch is taken out, and be obtained modified coal pitch to remove properties-correcting agent 3 times with the salt acid elution that concentration is 0.1mol/L.Accompanying drawing 3 is the microscopic optical structure of prepared modified coal pitch after 420 DEG C of carbonization 60min.
Embodiment 4
By anhydrous AlCl
3be crushed to particle diameter be below 0.1mm medium temperature coal pitch by weight 6wt%, in V-Mixer, mix 1h after send in reactor; Freely be warming up to 100 DEG C and be incubated half an hour, then 260 DEG C are warmed up to 5 DEG C/min temperature rise rate, and be incubated 5h, after cooling, modified coal-tar pitch is taken out, and be obtained modified coal pitch to remove properties-correcting agent 3 times with the salt acid elution that concentration is 0.1mol/L.Accompanying drawing 4 is the prepared microscopic optical structure of modified coal pitch after 420 DEG C of carbonization 60min.
Embodiment 5
By anhydrous AlCl
3be crushed to particle diameter be below 0.1mm medium temperature coal pitch by weight 2wt%, in V-Mixer, mix 1h after send in reactor; Freely be warming up to 100 DEG C and be incubated half an hour, then 260 DEG C are warmed up to 5 DEG C/min temperature rise rate, and be incubated 3h, after cooling, modified coal-tar pitch is taken out, and be obtained modified coal pitch to remove properties-correcting agent 3 times with the salt acid elution that concentration is 0.1mol/L.Accompanying drawing 5 is the prepared microscopic optical structure of modified coal pitch after 420 DEG C of carbonization 60min.
Embodiment six
By anhydrous AlCl
3be crushed to particle diameter be below 0.1mm medium temperature coal pitch by weight 10wt%, in V-Mixer, mix 1h after send in reactor; Freely be warming up to 100 DEG C and be incubated half an hour, then 260 DEG C are warmed up to 5 DEG C/min temperature rise rate, and be incubated 3h, after cooling, modified coal-tar pitch is taken out, and be obtained modified coal pitch to remove properties-correcting agent 3 times with the salt acid elution that concentration is 0.1mol/L.Accompanying drawing 6 is the prepared microscopic optical structure of modified coal pitch after 420 DEG C of carbonization 60min.
Accompanying drawing 1,2,3 represents identical modification dosage (6wt%) and under the reaction times (3h) respectively, the optical texture of modified coal pitch coking product prepared under different modification temperature (220 DEG C, 260 DEG C, 300 DEG C).Visible, at differential responses temperature, the optical texture of modified coal pitch coking product has obvious difference, and along with the rising of temperature of reaction, the structural area of the domain type of modified coal pitch first increases, rear reduction, and the area of mosaic structure first reduces, rear increase.
Accompanying drawing 2 and accompanying drawing 4 for reacting the optical texture of modified coal pitch coking product prepared by 3h and 5h at 260 DEG C, by accompanying drawing 2 can see its optical texture be mainly grow up in 60 μm, be wider than wide area type structure (FD) and the small part mosaic structure of 10 μm; Accompanying drawing 4 be mainly grow up in 60 μm, be wider than the wide area type structure (FD) of 10 μm, small part is streamlined (CFA) and part inlay type structure slightly.The visible increase along with modification time, modified coal pitch coking product anisotropy domain type structure increases, and mosaic structure reduces.
Accompanying drawing 2,5,6 represents identical modification temperature (260 DEG C) and under the reaction times (3h) respectively, the optical texture of the modified coal pitch coking product prepared by different properties-correcting agent usage quantity (6wt%, 2wt%, 10wt%).Visible, along with the increase of modification dosage, the area of the coking product anisotropy domain type structure of modified coal pitch first increases, rear minimizing, mosaic structure area first reduces, rear increase, this is because without properties-correcting agent time, coal tar pitch modification degree is not dark, the softening temperature of coal-tar pitch is lower, in, small molecules content is more, temperature flowing is better, be conducive to the movement of molecule, orientation, easy forming region type structure.Along with the increase of the amount of properties-correcting agent, the modification heighten degree of coal-tar pitch, in coal-tar pitch, the content of β resin increases, improve the temperature flowing of coal-tar pitch, be conducive to the nucleation of coal-tar pitch mesophase ball, grow up, melt also, organizer mesophase spherule, form the domain type structure of larger area, but the amount of properties-correcting agent is too high, make the softening temperature of modified coal pitch too high, temperature flowing is deteriorated, and a large amount of QI component generated, what hinder its mesophase spherule melts also, and mosaic structure increases, and domain type structure reduces.
By above-mentioned medium temperature coal pitch method of modifying, prepared modified coal pitch has following performance index:
1, softening temperature adopts GB/T4507-2014 method to record;
2, coking value adopts the coking value measuring method of GB/T8727-2008 coal-tar pitch to measure;
Table one is modification temperature 260 DEG C, and during modification 3h, the amount of anhydrous AlCl3 is on the impact of coal tar pitch soften point, coking value;
Table one
3, Group Component adopts GB2293-2008 method to record quinoline insolubles (QI) content is 5.73% ~ 17.20%; Adopting GB2292-1997 method to record toluene insolubles (BI) content is 20.02% ~ 45.17%, as anhydrous AlCl
3when add-on increases to 10% by 2%, TI-QS(β resin) content is increased to 26.24% by 15.66%; Table two is the performance of material asphalt.
Table two
As can be seen from above data, compare starting material pitch and heat-treat modifying asphalt, using anhydrous AlCl
3the coal-tar pitch of modification has higher softening temperature and coking value, especially find out that its β resin content has had from Group Component data significantly to improve, β resin is the presoma of mesophase spherule, the formation of mesophase spherule, the stratiform of condensation charcoal net is made to pile up ordering, the final easy graphitized charcoal forming ordered 3 D structure.From the formation of mesophase spherule, the Carbon Materials of stuctures and properties excellence can be prepared.
Above medium temperature coal pitch method of modifying of the present invention is described in detail.Apply specific case herein to set forth principle of the present invention and embodiment, the explanation of above embodiment just understands core concept of the present invention for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also belong in the protection domain of the claims in the present invention.
Claims (6)
1. a medium temperature coal pitch method of modifying, comprises the following steps:
(1) raw material mixing: anhydrous AlCl
3mix in mixer by weight 2 ~ 12wt% with medium temperature coal pitch; The time of mixing is 40-80min;
(2) react: step (1) gained mixing raw material is sent in reactor, passes into N
2get rid of the air in reactor, first temperature is risen to 95-105 DEG C, and is incubated 25-35min, then, then be warming up to 200 ~ 320 DEG C, reaction 1 ~ 5h, is cooled to room temperature;
(3) wash: by cooling gained crushing material after step (2) reaction, then wash with the dilute hydrochloric acid of 0.08-0.12mol/L, filter more than 2 times, vacuum-drying is to remove modifier A lCl
3and moisture, obtain modified medium temperature coal pitch.
2. a kind of medium temperature coal pitch method of modifying as claimed in claim 1, is characterized in that: described step (1) anhydrous AlCl
3purity is more than 98%.
3. a kind of medium temperature coal pitch method of modifying as claimed in claim 1 or 2, is characterized in that: anhydrous AlCl in described step (1)
3with medium temperature coal pitch by weight scope be 4 ~ 10wt%.
4. a kind of medium temperature coal pitch method of modifying as claimed in claim 1, is characterized in that: the N passed in described step (2)
2flow is 200ml/min, for getting rid of the air in reactor; The described temperature rise rate heated up again is 5-10 DEG C/min; The temperature of described reaction is 220 DEG C-300 DEG C, and soaking time is 2 ~ 5h.
5. a kind of medium temperature coal pitch method of modifying as claimed in claim 1, is characterized in that: number of times >=3 time of washing in described step (3).
6. modification medium temperature coal pitch as obtained in above-mentioned medium temperature coal pitch method of modifying, is characterized in that: described modification medium temperature coal pitch softening temperature is 98.6 ~ 152.2 DEG C; Coking value is 53.5 ~ 64.0%; Group Component quinoline insolubles QI content is 5.73% ~ 17.20%; Toluene insolubles BI content is 20.02% ~ 45.17%, β resin TI-QS content is 15.66 ~ 26.24%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109439004A (en) * | 2018-11-07 | 2019-03-08 | 平顶山东方碳素股份有限公司 | High temperature modified coal tar pitch and preparation method thereof |
| CN109971502A (en) * | 2019-04-19 | 2019-07-05 | 平顶山东方碳素股份有限公司 | A kind of anti-oxidant preparation process of adhesive coal tar pitch coking |
| CN112430095A (en) * | 2020-12-03 | 2021-03-02 | 中国科学院山西煤炭化学研究所 | Method for preparing high-performance graphite from graphene oxide modified coal pitch |
| CN116496087A (en) * | 2023-05-22 | 2023-07-28 | 湖南大学 | Superfine structure special carbon material and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109439004A (en) * | 2018-11-07 | 2019-03-08 | 平顶山东方碳素股份有限公司 | High temperature modified coal tar pitch and preparation method thereof |
| CN109439004B (en) * | 2018-11-07 | 2021-05-25 | 平顶山东方碳素股份有限公司 | High-temperature modified coal pitch and preparation method thereof |
| CN109971502A (en) * | 2019-04-19 | 2019-07-05 | 平顶山东方碳素股份有限公司 | A kind of anti-oxidant preparation process of adhesive coal tar pitch coking |
| CN112430095A (en) * | 2020-12-03 | 2021-03-02 | 中国科学院山西煤炭化学研究所 | Method for preparing high-performance graphite from graphene oxide modified coal pitch |
| CN116496087A (en) * | 2023-05-22 | 2023-07-28 | 湖南大学 | Superfine structure special carbon material and preparation method thereof |
| CN116496087B (en) * | 2023-05-22 | 2024-05-24 | 湖南大学 | Superfine structure special carbon material and preparation method thereof |
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