CN105170111A - Coal tar asphalt porous material and preparation method therefor and application thereof - Google Patents
Coal tar asphalt porous material and preparation method therefor and application thereof Download PDFInfo
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- CN105170111A CN105170111A CN201510438313.XA CN201510438313A CN105170111A CN 105170111 A CN105170111 A CN 105170111A CN 201510438313 A CN201510438313 A CN 201510438313A CN 105170111 A CN105170111 A CN 105170111A
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- porous material
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- tar pitch
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Abstract
The invention discloses a coal tar asphalt porous material and a preparation method therefor and application thereof, and relates to asphalt. The coal tar asphalt porous material is prepared from the following components in mass ratio: 1% of coal tar asphalt and 0.53-2.7% of a crosslinking agent. The preparation method for the coal tar asphalt porous material comprises the following steps: S1, firstly dissolving viscous coal tar asphalt in a solvent, then adding dimethoxymethane, and after uniform stirring, adding a crosslinking catalyst to obtain a mixed solution; S2, putting the mixed solution prepared in S1 into a reaction container, introducing argon, and after temperature-raising reaction, reducing the temperature to room temperature to obtain an asphalt-based porous material; S3, washing, extracting and drying the asphalt-based porous material obtained in S2 to obtain the coal tar asphalt porous material. The coal tar asphalt porous material can be applied to the field of preparing a gas adsorbent and a dye treatment agent and the like, and is mild in production condition, high in production efficiency and simple in process. The product asphalt porous material is large in specific surface area, and has relatively good gas adsorbing and storing performances; the asphalt porous material is low in cost and free of toxicity.
Description
Technical field
The present invention relates to pitch, especially relate to a kind of reaction with Friedel-Crafts and coal tar pitch and dimethoxymethane are cross-linked, a kind of coal tar pitch porous material that can obtain specific area large multi-orifice material and preparation method thereof and application.
Technical background
Pitch is the product obtained in Crude Oil Processing, is made up of the hydrocarbon and their derivative of different molecular weight.Coal tar pitch is the byproduct of coking, namely residual after tar distillation atrament, containing the aromatic hydrocarbon of the anthracene of volatilization in distress, pyrene and benzene class, so coal tar pitch has toxicity.As mineral waste, the utilization rate of coal tar pitch is not very high.
Porous carbon materials prepared by pitch, as active carbon etc.Chinese patent 98123530.1 discloses a kind of preparation method of mesopore asphalt-base globular active carbon.The method is flooded once activating the obtained asphalt-base globular active carbon with certain specific surface in the solution of the metallic compound such as frerrous chloride and cobalt chloride and drying, at 800 ~ 1000 DEG C, carry out re-activation with steam or carbon dioxide, obtained specific area is at 1000 ~ 1650m
2between/g, mesopore pore size is between 2 ~ 4nm, and total pore volume is between 0.22 ~ 0.58cm
3active carbon between/g.Chinese patent 200810037093.X discloses a kind of preparation method of high-carbon yield asphalt group spherical absorbent charcoal.The method by non-fusible bitumen ball being mixed with chemical activating agent zinc chloride or phosphoric acid solution, then is heated to 300-800 DEG C and carries out carbonization, activation, and after pickling, washing, obtained specific area is between 1100 ~ 1320m
2between/g, total pore volume is between 0.54 ~ 0.63cm
3asphalt-base spherical activated carbon between/g.Chinese patent 200910043229.2 announces a kind of preparation method of stored energy porous carbon materials.The method take specific area as 1100m
2the SO of/g
2for template, mesophase pitch is carbon source, pitch and SO
2electric furnace is put into, at N after mixing
2be incubated 8h after electric furnace being warming up to 300 DEG C under protection, after being then warming up to 900 DEG C, be incubated 1h, last N
2the lower cooling of protection, then remove SO with the hydrofluoric acid of 30%
2template, filters, is washed to neutrality, 100 DEG C of dryings, and obtained specific area is 600m
2the porous carbon of/g.Chinese patent 201510055624.8 discloses a kind of preparation method of mesopore asphaltic base shelly Carbon Materials.The method is that asphalt adds nano zine oxide ground and mixed, then adds the pulverous potassium hydroxide through grinding, and ground and mixed is even.This mixture is placed in tube furnace, in argon gas atmosphere, is heated to 200 DEG C with the heating rate of 5 DEG C/min, constant temperature 30min, is being heated to 800 ~ 900 DEG C, constant temperature 60min, naturally cool, the product obtained obtains specific area between 1766 ~ 2646m after pickling, washing and drying
2between/g, the shelly Mesoporous Carbon Materials of average pore size between 2.05 ~ 2.25nm.
It is carbon source that paper " Preparationofpitch-basedcarbonmaterialsusingatemplateand anorthogonalarraydesignforsupercapacitors " (Micro & NanoLetters12 (2014) 927-931) proposes with coal tar pitch, adopts different nano level oxide (ZrO
2, Al
2o
3, TiO
2) as template.Coal tar pitch and oxide mixing, at the N of 50ml/min
2under atmosphere, be warming up to 500 DEG C of insulation 2h with the heating rate of 5 DEG C/min, naturally cool to room temperature, add KOH mixing, at 700 ~ 900 DEG C, be incubated 90min, after the sulfuric acid of the product 6mol/L obtained washes away template, washing, 110 DEG C of dry 4h.Obtain specific area at 935 ~ 2071m
2between/g, pore volume is at 0.58 ~ 1.16cm
3material with carbon element between/g.It is carbon source that paper " Preparationofmesophasepitchbasedmesoporouscarbonsusingan imprintingmethod " (Newcarbonmaterials22 (2007) 259-263) proposes with mesophase pitch, and nanometer silica gel is that perforating agent adopts print process to prepare mesoporous carbon.After mesophase pitch and silica gel mix and blend 5h, at 900 DEG C of charing 2h after 340 ~ 400 DEG C of heat treatment 2h, gained mixture 3M sodium hydroxide solution repeatedly washs 2h in 94 DEG C, then at room temperature wash 12h removing silica gel pattern mould with the hydrofluoric acid of 37%, the specific area of gained coal tar pitch base mesoporous carbon is 140m
2/ g, its total pore volume is 0.31cm
3/ g.Paper " preparation of template coal tar pitch base mesoporous carbon and chemical property thereof " (novel charcoal material, 26 (2011) 187-191) propose with coal tar pitch to be carbon source, with silica be template adopt vapor phase method prepare Mesoporous Carbon Materials, coal tar pitch and silica quality ratio be 1: 1.2 mixture with six sections of temperature programmings, mixture is heated after 5h stirs, subsequently, pass into carbon dioxide at 900 DEG C to activate, finally obtain mesoporous carbon by hydrofluoric acid wash activation products; Wherein, soak time is when 90 ~ 150min, and the specific area of gained mesoporous carbon is between 830 ~ 1360m
2between/g.
As can be seen from above-mentioned patent and document, take mesophase pitch as carbon source, silica or silica gel etc. are template, need hydrofluoric acid to remove template, and operation is comparatively complicated and seriously polluted; Take asphalt as carbon source, adopt hard template or chemical activation method by adding the technique of hot preparation porous carbon, its soak time is long, and energy consumption is high, and cost is high, seriously polluted.Hole as much higher in obtained specific area material with carbon element, needs the condition of HTHP, high to equipment requirement, poor safety performance.These problem all limits the development that pitch prepares the porous materials such as active carbon.
Summary of the invention
For above shortcomings in existing pitch porous material technology of preparing, the present invention aims to provide that can to obtain specific area large, performance is excellent, the asphaltic base porous material of good cycling stability, reaction condition is gentle, and cost is low, and equipment investment is few, technological difficulty is low, a kind of coal tar pitch porous material that product competitiveness is higher and preparation method thereof and application.
Described coal tar pitch porous material consisting of in mass ratio: coal tar pitch 1, crosslinking agent 0.53 ~ 2.7.
Described crosslinking agent can adopt dimethoxymethane etc.
The preparation method of described coal tar pitch porous material is as follows:
1) thick coal tar pitch is first dissolved in a solvent, then add dimethoxymethane, after stirring, add crosslinking catalyst, obtain mixed solution;
2) by step 1) mixed solution prepared puts into reaction vessel, and pass into argon gas, after temperature reaction, be cooled to room temperature, obtain asphaltic base porous material;
3) by step 2) cleaning of the asphaltic base porous material that obtains, extracting, dries, obtains coal tar pitch porous material.
In step 1) in, described solvent can adopt 1,2-dichloroethanes etc., and described 1,2-dichloroethanes preferably adopts 1,2-dichloroethanes of purifying; Described crosslinking catalyst can adopt anhydrous ferric trichloride etc.
In step 2) in, the temperature of described temperature reaction can be 80 DEG C, and the time of temperature reaction can be 8h.
In step 3) in, described cleaning can adopt washed with methanol 3 times; Described extracting first can use methyl alcohol extracting 5h, then uses carrene extracting 5h; The temperature of described oven dry can be 80 DEG C, and the time of oven dry can be 12h.
Obtained coal tar pitch porous material application testing is as follows: under pressure 1.13bar, temperature 77K, test N respectively
2absorption, tests CO under pressure 1.0bar, temperature 273.15K
2absorption.
Described coal tar pitch porous material can be applied preparing in the field such as adsorbent and dyestuff inorganic agent.
Advantage of the present invention and good effect:
1. formula for raw stock involved in the present invention is for production equipment without particular/special requirement, and working condition is gentle, and production efficiency is high, and technique is simple.
2. the pitch porous material produced of the present invention, specific area is large, has good gas absorption and storge quality.
3. through the super crosslinked coal tar pitch porous material of Friedel-Crafts, compared with the porous materials such as active carbon general on the market, cost is low, nontoxic, make the utilization of coal tar pitch more extensive, it can be extended to exhaust-gas treatment in enterprise or life better, energy storage, in the application such as dyestuff process.
Accompanying drawing explanation
Fig. 1 is the nitrogen Adsorption and desorption isotherms of asphaltic base porous material prepared by the embodiment of the present invention 1 ~ 4.
Fig. 2 is the CO of asphaltic base porous material prepared by the embodiment of the present invention 1 ~ 4
2adsorbance curve.
Detailed description of the invention
Embodiment 1
Preparation specific area is 540m
2/ g, pore volume is 0.23cm
3the super cross-linked bitumen porous material of/g.
The present embodiment adopts following formula:
Coal tar pitch: 1.00g
Dimethoxymethane: 0.53g
Anhydrous ferric trichloride: 2.29g
1,2-dichloroethanes: 10ml
Pitch porous material is prepared in accordance with the following methods with above-mentioned compound composition:
1. first the coal tar pitch taken is dissolved in 1,2-dichloroethanes, to be dissolved completely after, add dimethoxymethane, be uniformly mixed, add anhydrous ferric trichloride, mix.
2. by the composition that mixes under an argon atmosphere, be heated to 80 DEG C, crosslinked 8h.
3. by the solid of step 2 gained, first wash away part ferric trichloride with methyl alcohol, then use methyl alcohol extracting 5h, then use carrene extracting 5h instead, dry 12h for latter 80 DEG C.
Embodiment 2
Preparation specific area is 447m
2/ g, pore volume is 0.19cm
3the super cross-linked bitumen porous material of/g.
The present embodiment adopts following formula:
Coal tar pitch: 1.00g
Dimethoxymethane: 0.88g
Anhydrous ferric trichloride: 3.80g
1,2-dichloroethanes: 10ml
Pitch porous material is prepared in accordance with the following methods with above-mentioned compound composition:
1. first the coal tar pitch taken is dissolved in 1,2-dichloroethanes, to be dissolved completely after, add dimethoxymethane, be uniformly mixed, add anhydrous ferric trichloride, mix.
2. by the composition that mixes under an argon atmosphere, be heated to 80 DEG C, crosslinked 8h.
3. by the solid of step 2 gained, first wash away part ferric trichloride with methyl alcohol, then use methyl alcohol extracting 5h, then use carrene extracting 5h instead, dry 12h for latter 80 DEG C.
Embodiment 3
Preparation specific area is 493m
2/ g, pore volume is 0.21cm
3the super cross-linked bitumen porous material of/g.
The present embodiment adopts following formula:
Coal tar pitch: 1.00g
Dimethoxymethane: 1.34g
Anhydrous ferric trichloride: 5.70g
1,2-dichloroethanes: 10ml
Pitch porous material is prepared in accordance with the following methods with above-mentioned compound composition:
1. first the coal tar pitch taken is dissolved in 1,2-dichloroethanes, to be dissolved completely after, add dimethoxymethane,
Be uniformly mixed, add anhydrous ferric trichloride, mix.
2. by the composition that mixes under an argon atmosphere, be heated to 80 DEG C, crosslinked 8h.
3. by the solid of step 2 gained, first wash away part ferric trichloride with methyl alcohol, then use methyl alcohol extracting 5h, then use dichloro instead
Methane extracting 5h, dries 12h for latter 80 DEG C.
Embodiment 4
Preparation specific area is 425m
2/ g, pore volume is 0.18cm
3the super cross-linked bitumen porous material of/g.
The present embodiment adopts following formula:
Coal tar pitch: 1.00g
Dimethoxymethane: 2.68g
Anhydrous ferric trichloride: 11.43g
1,2-dichloroethanes: 10ml
Pitch porous material is prepared in accordance with the following methods with above-mentioned compound composition:
1. first the coal tar pitch taken is dissolved in 1,2-dichloroethanes, to be dissolved completely after, add dimethoxymethane, be uniformly mixed, add anhydrous ferric trichloride, mix.
2. by the composition that mixes under an argon atmosphere, be heated to 80 DEG C, crosslinked 8h.
3. by the solid of step 2 gained, first wash away part ferric trichloride with methyl alcohol, then use methyl alcohol extracting 5h, then use carrene extracting 5h instead, dry 12h for latter 80 DEG C.
The pore structure parameter of embodiment 1 ~ 4 gained asphaltic base porous material and CO
2the summarized results of Adsorption test data lists in table 1.
Table 1
The nitrogen Adsorption and desorption isotherms of asphaltic base porous material prepared by the embodiment of the present invention 1 ~ 4 see Fig. 1, the CO of asphaltic base porous material prepared by the embodiment of the present invention 1 ~ 4
2adsorbance curve is see Fig. 2.
The present invention take coal tar pitch as substrate raw material, adopt the super crosslinked explained hereafter asphaltic base porous material of Friedel-Crafts, raw material makes substrate raw material and external crosslinker generation cross-linking reaction by Friedel-Crafts, carries out super crosslinked, can generate three-dimensional porous material.The specific area of this asphaltic base porous material is at 425 ~ 540m
2between/g, pore volume is at 0.18 ~ 0.23cm
3between/g.The main feature of this process is that equipment investment is few, and production process is easy, and production efficiency is high, and cost is low is conducive to large-scale production and popularization.Poisonous coal tar pitch is used to prepare the asphaltic base porous material of nonhazardous, not only in coal tar pitch utilizes, expand the scope of application, and obtained three-dimensional porous material has good gas absorption and storge quality, to the absorption of dyestuff and the efficient performance of process, will have broad application prospects after making the after-treatment of coal tar pitch.
Claims (10)
1. a coal tar pitch porous material, is characterized in that its consisting of in mass ratio: coal tar pitch 1, crosslinking agent 0.53 ~ 2.7.
2. a kind of coal tar pitch porous material as claimed in claim 1, is characterized in that described crosslinking agent adopts dimethoxymethane.
3. the preparation method of a kind of coal tar pitch porous material as claimed in claim 1, is characterized in that comprising the following steps:
1) thick coal tar pitch is first dissolved in a solvent, then add dimethoxymethane, after stirring, add crosslinking catalyst, obtain mixed solution;
2) by step 1) mixed solution prepared puts into reaction vessel, and pass into argon gas, after temperature reaction, be cooled to room temperature, obtain asphaltic base porous material;
3) by step 2) cleaning of the asphaltic base porous material that obtains, extracting, dries, obtains coal tar pitch porous material.
4. the preparation method of a kind of coal tar pitch porous material as claimed in claim 3, is characterized in that in step 1) in, described solvent adopts 1,2-dichloroethanes.
5. the preparation method of a kind of coal tar pitch porous material as claimed in claim 4, is characterized in that described 1,2-dichloroethanes adopts 1,2-dichloroethanes of purifying.
6. the preparation method of a kind of coal tar pitch porous material as claimed in claim 3, is characterized in that in step 1) in, described crosslinking catalyst adopts anhydrous ferric trichloride.
7. the preparation method of a kind of coal tar pitch porous material as claimed in claim 3, is characterized in that in step 2) in, the temperature of described temperature reaction is 80 DEG C, and the time of temperature reaction is 8h.
8. the preparation method of a kind of coal tar pitch porous material as claimed in claim 3, is characterized in that in step 3) in, described cleaning adopts washed with methanol 3 times; Described extracting first can use methyl alcohol extracting 5h, then uses carrene extracting 5h.
9. the preparation method of a kind of coal tar pitch porous material as claimed in claim 3, is characterized in that in step 3) in, the temperature of described oven dry is 80 DEG C, and the time of oven dry is 12h.
10. coal tar pitch porous material is applied preparing in adsorbent and dyestuff inorganic agent as claimed in claim 1.
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|---|---|---|---|
| CN201510438313.XA CN105170111A (en) | 2015-07-23 | 2015-07-23 | Coal tar asphalt porous material and preparation method therefor and application thereof |
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| CN201510438313.XA CN105170111A (en) | 2015-07-23 | 2015-07-23 | Coal tar asphalt porous material and preparation method therefor and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107871615A (en) * | 2016-09-27 | 2018-04-03 | 国家纳米科学中心 | A kind of porous carbon nanomaterial and its production and use |
| CN108126722A (en) * | 2018-01-31 | 2018-06-08 | 宁夏大学 | A kind of coal base W/WC composite catalysts and preparation method thereof |
| CN108517051A (en) * | 2018-04-09 | 2018-09-11 | 厦门大学 | Coal tar pitch porous polymer and preparation method and application prepared by heteropoly acid catalysis |
| CN111072009A (en) * | 2019-12-25 | 2020-04-28 | 大连理工大学 | Hard carbon material and preparation method and application thereof |
| CN112850705A (en) * | 2020-07-04 | 2021-05-28 | 山东八三石墨新材料厂 | Method for preparing electrode material of super capacitor by using asphalt as raw material |
| CN113967461A (en) * | 2020-07-24 | 2022-01-25 | 中国石油化工股份有限公司 | Amino-rich porous carbon material and preparation method and application thereof |
| CN114433027A (en) * | 2020-11-02 | 2022-05-06 | 中国石油化工股份有限公司 | Solid amine modified porous material and preparation method thereof |
| CN115715977A (en) * | 2022-11-15 | 2023-02-28 | 湖南科技大学 | Asphalt-based magnetic HCPs adsorbent and preparation method and application thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107871615A (en) * | 2016-09-27 | 2018-04-03 | 国家纳米科学中心 | A kind of porous carbon nanomaterial and its production and use |
| CN108126722A (en) * | 2018-01-31 | 2018-06-08 | 宁夏大学 | A kind of coal base W/WC composite catalysts and preparation method thereof |
| CN108517051A (en) * | 2018-04-09 | 2018-09-11 | 厦门大学 | Coal tar pitch porous polymer and preparation method and application prepared by heteropoly acid catalysis |
| CN111072009A (en) * | 2019-12-25 | 2020-04-28 | 大连理工大学 | Hard carbon material and preparation method and application thereof |
| CN112850705A (en) * | 2020-07-04 | 2021-05-28 | 山东八三石墨新材料厂 | Method for preparing electrode material of super capacitor by using asphalt as raw material |
| CN113967461A (en) * | 2020-07-24 | 2022-01-25 | 中国石油化工股份有限公司 | Amino-rich porous carbon material and preparation method and application thereof |
| CN113967461B (en) * | 2020-07-24 | 2023-07-21 | 中国石油化工股份有限公司 | Porous carbon material rich in amino groups and preparation method and application thereof |
| CN114433027A (en) * | 2020-11-02 | 2022-05-06 | 中国石油化工股份有限公司 | Solid amine modified porous material and preparation method thereof |
| CN114433027B (en) * | 2020-11-02 | 2024-02-13 | 中国石油化工股份有限公司 | Solid amine modified porous material and preparation method thereof |
| CN115715977A (en) * | 2022-11-15 | 2023-02-28 | 湖南科技大学 | Asphalt-based magnetic HCPs adsorbent and preparation method and application thereof |
| CN115715977B (en) * | 2022-11-15 | 2023-05-16 | 湖南科技大学 | Asphalt-based magnetic HCPs adsorbent and preparation method and application thereof |
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