CN104148031A - Method for preparing poly-dopamine carbon material with high specific surface area - Google Patents
Method for preparing poly-dopamine carbon material with high specific surface area Download PDFInfo
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- CN104148031A CN104148031A CN201410369865.5A CN201410369865A CN104148031A CN 104148031 A CN104148031 A CN 104148031A CN 201410369865 A CN201410369865 A CN 201410369865A CN 104148031 A CN104148031 A CN 104148031A
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Abstract
The invention discloses a method for preparing a poly-dopamine carbon material with high specific surface area. The method comprises the following steps: (1) dissolving dopamine hydrochloride in deionized water to obtain a dopamine hydrochloride aqueous solution, and pouring the dopamine hydrochloride aqueous solution into a mixed solution of ethyl alcohol and ammonia water; and putting in a closed container and fully stirring to obtain a poly-dopamine ball mixed solution, and filtering, flushing and drying the obtained poly-dopamine ball mixed solution to obtain solid poly-dopamine balls; and (2) mixing the solid poly-dopamine balls with KOH, fully mixing and grinding, conducting high-temperature activating reaction in the Ar atmosphere, and then washing, filtering and drying to obtain the poly-dopamine carbon material with the high specific surface area. The poly-dopamine porous carbon material prepared by the method has the characteristics of simple process, high yield and specific surface area and large pore volume, and the pore structure of the poly-dopamine carbon material can be regulated by regulating the amount of KOH. Materials with different specific surface areas and pore volumes are synthesized to obtain the poly-dopamine carbon material with high specific surface area and large pore volume.
Description
Technical field
The present invention relates to a kind of preparation method of the sorbing material with flourishing pore structure, be specifically related to a kind of high-ratio surface and gather the preparation method of dopamine material with carbon element.
Background technology
Dopamine is a kind of biomolecule of high carbon containing, extensively exists in biological shell top layer, is the carbon source material that mankind's sustainable (renewable) obtain.Dopamine can aggregate into dopamine ball under certain pH condition, will gather after dopamine ball warp is crossed carbonization treatment and obtain poly-dopamine material with carbon element.Poly-dopamine material with carbon element is with its pore structure prosperity, and hydrothermal stability is good, causes concern in fields such as the finishinges of catalysis material, membrane material and electrode material.Lu et al. (Kelong Ai, Yanlan Liu, Changping Ruan, Lehui Lu*and Gaoqing (Max) Lu*.Sp2 C-Dominant N-Doped Carbon Sub-micrometer Spheres with a Tunable Size:A Versatile Platform for Highly Efficient Oxygen-Reduction Catalysts.Adv.Mater.2013, 25, 998 – 1003) report a kind of synthetic method of poly-dopamine material with carbon element: (1) first will gather dopamine ball and under 800 degrees Celsius, carry out carbonization: mix with KOH the poly-dopamine ball after carbonization (2) with 1:4, then at 770 DEG C, carry out pyroreaction, finally obtain the poly-dopamine porous carbon materials of pore structure prosperity, its BET specific area is 2006 m
2/ g.This preparation method can be described as carbonization-activation method.
The method still has the following disadvantages:
1. material yield is too low;
2. its specific area of prepared material, pore volume still need further raising;
3. synthetic energy consumption is still higher, and it needs two high-temperature reaction process.
For above problem, the present invention proposes the poly-dopamine porous carbon materials of a kind of one-step method preparation.Not only can improve yield, can shorten again technique and reduce energy consumption and can make material there is higher specific area.
Summary of the invention:
The object of the invention is to the deficiency for aspects such as existing poly-dopamine material with carbon element hole mechanism and synthesis yields, propose a kind of more high-specific surface area and the more method of the poly-dopamine material with carbon element of large pore volume of synthesizing in the time reducing energy consumption, improve yield.
Object of the present invention is achieved through the following technical solutions:
High-ratio surface gathers a preparation method for dopamine material with carbon element, comprises the steps:
(1) Dopamine hydrochloride is dissolved in deionized water, obtains the Dopamine hydrochloride aqueous solution, then inject the mixed liquor of ethanol and ammoniacal liquor; Be placed in closed container and fully stir, obtain poly-dopamine ball mixed liquor, the poly-dopamine ball mixed liquor of gained is filtered, rinse, dry, obtain the poly-dopamine ball of solid;
(2) poly-the solid of step (1) gained dopamine ball and KOH are mixed, fully mixed grinding, carries out high-temperature activation reaction in Ar atmosphere, obtains the poly-dopamine material with carbon element of high-specific surface area after then cleaning, filter, drying.
In said method, in step (1), the described Dopamine hydrochloride aqueous solution is 1:50～200 configurations by the mass ratio of Dopamine hydrochloride crystal and deionized water, described Dopamine hydrochloride solution and ethanol and ammoniacal liquor are Dopamine hydrochloride solution according to volume ratio: ethanol: ammoniacal liquor=50～200:40:1, described stirring is at room temperature stirring 10～30h.
In said method, the poly-dopamine ball of solid described in step (2) and KOH mixed proportion are mass ratio 1:1～1:7, the reaction temperature of described high-temperature activation reaction is 500～800 DEG C, and the reaction time is 1～3h, and described cleaning is for using watery hydrochloric acid and deionized water rinsing 4 times; Described oven dry is 50 DEG C of-80 DEG C of vacuum drying.
In said method, the BET specific area of the poly-dopamine material with carbon element of described high-specific surface area is 2343-3534m
2/ g, total pore volume is 1.37-2.23cm
3/ g, wherein Micropore volume is 0.81-1.23cm
3/ g; The poly-dopamine material with carbon element of described high-specific surface area is coccoid structure, and particle diameter is within the scope of 300-600nm.
Compared with prior art, synthetic method advantage of the present invention:
1. save high temperature cabonization step, and adopted direct activation method, Energy Intensity Reduction approximately 50% left and right;
2. saved high temperature cabonization step, can greatly reduce again carbon loss, yield improves more than 50%;
3. the amount of regulation and control KOH can regulate the pore structure of poly-dopamine material with carbon element, synthesizes the different poly-dopamine material with carbon element of specific area and pore volume, can obtain more high-specific surface area and pore volume poly-dopamine material with carbon element.
Brief description of the drawings
The N of 4 kinds of different poly-dopamine material with carbon elements that Fig. 1 obtains for 4 kinds of embodiment of the present invention
2adsorption isotherm.
Fig. 2 is the preparation-obtained poly-dopamine porous carbon materials SEM figure of embodiment 1.
Fig. 3 is the preparation-obtained poly-dopamine porous carbon materials SEM figure of embodiment 2.
Fig. 4 is the preparation-obtained poly-dopamine porous carbon materials SEM figure of embodiment 3.
Fig. 5 is the preparation-obtained poly-dopamine porous carbon materials SEM figure of embodiment 4.
Detailed description of the invention
Below in conjunction with drawings and Examples, the invention will be further described, but the scope of protection of present invention is not limited to the scope of embodiment statement.
Embodiment 1
The Dopamine hydrochloride of 1g is dissolved in 50ml deionized water, this solution is poured in the mixed liquor that adds 40ml absolute ethyl alcohol and 0.75ml ammoniacal liquor (mass fraction 28%).Add rear sealing fully to stir 10h, just obtain poly-dopamine ball mixed liquor, by product filtering with microporous membrane, resulting materials is rinsed well by deionized water, and 50 degrees Celsius of vacuum drying 10h obtain the poly-dopamine ball of solid.Be that 1:1 mixes by poly-dopamine ball and KOH mass ratio, then fully mix and grind to stir and make it even, then put this solid mixture into tube furnace, under the atmosphere of Ar, be raised to 500 degrees Celsius with the heating rate of 5K/min, and maintain 500 degrees Celsius of 1h, until being naturally down to after room temperature, gained solid is dissolved in the HCl of 1mol/L, unreacted KOH is fully neutralized, repeatedly clean to pH=7 with filtering with microporous membrane and by deionized water again, 50 degrees Celsius of vacuum drying 12h, obtain the poly-dopamine porous carbon materials of solid.
Embodiment 2
The Dopamine hydrochloride of 1g is dissolved in 150ml deionized water, this solution is poured in the mixed liquor that adds 40ml absolute ethyl alcohol and 0.75ml ammoniacal liquor (28%).Add rear sealing fully to stir 15h, just obtain poly-dopamine ball mixed liquor, by product filtering with microporous membrane, resulting materials is rinsed well by deionized water, and 50 degrees Celsius of vacuum drying 10h obtain the poly-dopamine ball of solid.Be that 1:5 mixes by poly-dopamine ball and KOH mass ratio, then fully mix and grind to stir and make it even, then put this solid mixture into tube furnace, under the atmosphere of Ar, be raised to 700 degrees Celsius with the heating rate of 5K/min, and maintain 700 degrees Celsius of 2.5h, until being naturally down to after room temperature, gained solid is dissolved in the HCl of 1mol/L, unreacted KOH is fully neutralized, repeatedly clean to PH=7 with filtering with microporous membrane and by deionized water again, 60 degrees Celsius of vacuum drying 12h, obtain the poly-dopamine porous carbon materials of solid.
Embodiment 3
The Dopamine hydrochloride of 1g is dissolved in 100ml deionized water, this solution is poured in the mixed liquor that adds 40ml absolute ethyl alcohol and 0.75ml ammoniacal liquor (28%).Add rear sealing fully to stir 25h, just obtain poly-dopamine ball mixed liquor, by product filtering with microporous membrane, resulting materials is rinsed well by deionized water, and 50 degrees Celsius of vacuum drying 10h obtain the poly-dopamine ball of solid.Be that 1:3 mixes by poly-dopamine ball and KOH mass ratio, then fully mix and grind to stir and make it even, then put this solid mixture into tube furnace, under the atmosphere of Ar, be raised to 600 degrees Celsius with the heating rate of 5K/min, and maintain 600 degrees Celsius of 1.5h, until being naturally down to after room temperature, gained solid is dissolved in the HCl of 1mol/L, unreacted KOH is fully neutralized, repeatedly clean to PH=7 with filtering with microporous membrane and by deionized water again, 70 degrees Celsius of vacuum drying 12h, obtain the poly-dopamine porous carbon materials of solid.
Embodiment 4
The Dopamine hydrochloride of 1g is dissolved in 200ml deionized water, this solution is poured in the mixed liquor that adds 40ml absolute ethyl alcohol and 0.75ml ammoniacal liquor (28%).Add rear sealing fully to stir 30h, just obtain poly-dopamine ball mixed liquor, by product filtering with microporous membrane, resulting materials is rinsed well by deionized water, and 50 degrees Celsius of vacuum drying 10h obtain the poly-dopamine ball of solid.Be that 1:7 mixes by poly-dopamine ball and KOH mass ratio, then fully mix and grind to stir and make it even, then put this solid mixture into tube furnace, under the atmosphere of Ar, be raised to 800 degrees Celsius with the heating rate of 5K/min, and maintain 800 degrees Celsius of 3h, until being naturally down to after room temperature, gained solid is dissolved in the HCl of 1mol/L, unreacted KOH is fully neutralized, repeatedly clean to PH=7 with filtering with microporous membrane and by deionized water again, 80 degrees Celsius of vacuum drying 12h, obtain the poly-dopamine porous carbon materials of solid.
(1) the pore structure character of poly-dopamine material with carbon element
The ASAP-2020 specific surface pore-size distribution instrument that adopts Micro company of the U.S. to produce characterizes pore structure and the crystal structure of the prepared poly-dopamine material with carbon element of the present invention, and result is as shown in Fig. 1 and table 1.
Specific area and the pore structure of the poly-dopamine material with carbon element of four kinds of embodiment gained of table 1..
Fig. 1 is the N2 adsorption isotherms of four kinds of different embodiment under 77K condition, can be obtained by interpretation software processing the information such as specific area, pore volume of different embodiment according to thermoisopleth.As we can see from the figure along with the increase of activator level and the BET specific area first increases and then decreases of reaction temperature rising material and pore volume increases gradually.The BET specific area of the prepared poly-dopamine material with carbon element of the present invention is about 2343-3534m
2/ g, total pore volume scope is 1.37-2.23cm
3/ g, wherein Micropore volume is about 0.81-1.23cm
3/ g left and right; This illustrate four kinds of embodiment aperture structures of the present invention and specific area coverage very large; Poly-dopamine material with carbon element of the present invention has very large (in table 1) of more micropore and specific area and pore volume.
(2) SEM of poly-dopamine material with carbon element
Adopt Dutch FEI Quanta200 type low power SEM the prepared poly-dopamine material with carbon element of four kinds of embodiment of the present invention to be carried out to the sign of material surface pattern, operating condition is: under 35kV and 25mA, apply Cu K α
1ray (λ=1.54056) is measured.
From Fig. 2-Fig. 5, can see that four kinds of prepared poly-dopamine material with carbon elements of different embodiment have all kept good coccoid structure, bead size uniform is all between 300-600nm.
(3) yield of poly-dopamine material with carbon element
The yield contrast of the poly-dopamine material with carbon element of four kinds of different embodiment gained of table 2. and bibliographical information.
Table 2 is yield tables of the poly-dopamine material with carbon element of four kinds of different embodiment gained, and in table, the computational methods of yield are as follows:
Wherein m
ofor the quality of Dopamine hydrochloride, m
tfor the quality of the poly-dopamine material with carbon element of gained.
The yield of the poly-dopamine material with carbon element of documents report, the yield of the present invention's direct step activation method used is that 8%-11% is all higher than 3% of bibliographical information.
The above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also giving exhaustive to all embodiments.All any amendments of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in the protection domain of the claims in the present invention.
Claims (4)
1. a method of preparing the poly-dopamine material with carbon element of high-specific surface area, is characterized in that comprising the steps:
(1) Dopamine hydrochloride is dissolved in deionized water, obtains the Dopamine hydrochloride aqueous solution, then inject the mixed liquor of ethanol and ammoniacal liquor; Be placed in closed container and fully stir, obtain poly-dopamine ball mixed liquor, the poly-dopamine ball mixed liquor of gained is filtered, rinse, dry, obtain the poly-dopamine ball of solid;
(2) poly-the solid of step (1) gained dopamine ball and KOH are mixed, fully mixed grinding, carries out high-temperature activation reaction in Ar atmosphere, obtains the poly-dopamine material with carbon element of high-specific surface area after then cleaning, filter, drying.
2. the preparation method of the poly-dopamine material with carbon element of high-specific surface area according to claim 1, it is characterized in that, in step (1), the described Dopamine hydrochloride aqueous solution is 1:50 ~ 200 configurations by the mass ratio of Dopamine hydrochloride crystal and deionized water, described Dopamine hydrochloride solution and ethanol and ammoniacal liquor are Dopamine hydrochloride solution according to volume ratio: ethanol: ammoniacal liquor=50 ~ 200: 40:1, described stirring is at room temperature stirring 10 ~ 30 h.
3. the preparation method of the poly-dopamine material with carbon element of high-specific surface area according to claim 1, it is characterized in that, the poly-dopamine ball of solid described in step (2) and KOH mixed proportion are mass ratio 1:1 ~ 1:7, the reaction temperature of described high-temperature activation reaction is 500 ~ 800 DEG C, reaction time is 1 ~ 3h, and described cleaning is for using watery hydrochloric acid and deionized water rinsing 4 times; Described oven dry is 50 DEG C of-80 DEG C of vacuum drying.
4. the preparation method of the poly-dopamine material with carbon element of high-specific surface area according to claim 1, is characterized in that, the BET specific area of the poly-dopamine material with carbon element of described high-specific surface area is 2343-3534 m
2/ g, total pore volume is 1.37-2.23 cm
3/ g, wherein Micropore volume is 0.81-1.23 cm
3/ g; The poly-dopamine material with carbon element of described high-specific surface area is coccoid structure, and particle diameter is within the scope of 300-600 nm.
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|---|---|---|---|---|
| CN105289540A (en) * | 2015-11-11 | 2016-02-03 | 江苏大学 | Method for preparing porous difunctional adsorption material |
| CN105289688A (en) * | 2015-11-03 | 2016-02-03 | 安徽师范大学 | Method for preparing oxygen reduction catalyst transition metallic oxide/nitrogen-doped carbon composite material |
| CN105664936A (en) * | 2016-01-07 | 2016-06-15 | 上海工程技术大学 | Method for preparing nano composite material having core-shell structure with dopamine as carbon source |
| CN107057326A (en) * | 2017-02-16 | 2017-08-18 | 四川大学 | Composite of photoresponse shape memory selfreparing and preparation method thereof, restorative procedure and application |
| CN107442084A (en) * | 2017-07-26 | 2017-12-08 | 华南理工大学 | A kind of poly-dopamine pitch base composite porous carbon adsorbing material of Preferential adsorption ethane and preparation method and application |
| CN107697912A (en) * | 2017-09-30 | 2018-02-16 | 青岛大学 | A kind of preparation method of biomass-based porous agraphitic carbon nanosphere electrode material |
| CN110152611A (en) * | 2019-07-04 | 2019-08-23 | 浙江海洋大学 | A kind of preparation method of adsorbent material |
| CN110305634A (en) * | 2019-07-04 | 2019-10-08 | 浙江海洋大学 | A kind of preparation method of carbon ball base composite phase-change material |
| CN110527493A (en) * | 2019-07-04 | 2019-12-03 | 浙江海洋大学 | A kind of preparation method of shaping phase-change material |
| CN110527494A (en) * | 2019-07-04 | 2019-12-03 | 浙江海洋大学 | A kind of preparation method of the mesoporous compound organic phase change material of silicon substrate high thermal conductivity |
| CN111530424A (en) * | 2020-06-17 | 2020-08-14 | 福州大学 | Copper-loaded modified carbon material adsorbent for efficiently removing gaseous benzene series and preparation method and application thereof |
| CN112452355A (en) * | 2020-12-10 | 2021-03-09 | 浙江海洋大学 | Preparation method of carbon material catalyst applied to styrene preparation |
| CN113231014A (en) * | 2021-04-12 | 2021-08-10 | 东南大学 | Hydrophobic biomass polydopamine composite activated carbon and preparation method thereof |
| CN113368826A (en) * | 2021-07-06 | 2021-09-10 | 江阴市锦绣江南环境发展有限公司 | Adsorbent for heavy metal wastewater treatment and preparation method thereof |
| CN117384647A (en) * | 2023-12-11 | 2024-01-12 | 同济大学 | Furillic acid composite nitrogen-doped magnetic carbon submicron sphere and preparation method and application thereof |
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| CN105289688A (en) * | 2015-11-03 | 2016-02-03 | 安徽师范大学 | Method for preparing oxygen reduction catalyst transition metallic oxide/nitrogen-doped carbon composite material |
| CN105289540A (en) * | 2015-11-11 | 2016-02-03 | 江苏大学 | Method for preparing porous difunctional adsorption material |
| CN105289540B (en) * | 2015-11-11 | 2017-07-18 | 江苏大学 | A kind of method for preparing porous difunctional sorbing material |
| CN105664936A (en) * | 2016-01-07 | 2016-06-15 | 上海工程技术大学 | Method for preparing nano composite material having core-shell structure with dopamine as carbon source |
| CN107057326A (en) * | 2017-02-16 | 2017-08-18 | 四川大学 | Composite of photoresponse shape memory selfreparing and preparation method thereof, restorative procedure and application |
| CN107442084A (en) * | 2017-07-26 | 2017-12-08 | 华南理工大学 | A kind of poly-dopamine pitch base composite porous carbon adsorbing material of Preferential adsorption ethane and preparation method and application |
| CN107697912A (en) * | 2017-09-30 | 2018-02-16 | 青岛大学 | A kind of preparation method of biomass-based porous agraphitic carbon nanosphere electrode material |
| CN110305634A (en) * | 2019-07-04 | 2019-10-08 | 浙江海洋大学 | A kind of preparation method of carbon ball base composite phase-change material |
| CN110152611A (en) * | 2019-07-04 | 2019-08-23 | 浙江海洋大学 | A kind of preparation method of adsorbent material |
| CN110527493A (en) * | 2019-07-04 | 2019-12-03 | 浙江海洋大学 | A kind of preparation method of shaping phase-change material |
| CN110527494A (en) * | 2019-07-04 | 2019-12-03 | 浙江海洋大学 | A kind of preparation method of the mesoporous compound organic phase change material of silicon substrate high thermal conductivity |
| CN111530424A (en) * | 2020-06-17 | 2020-08-14 | 福州大学 | Copper-loaded modified carbon material adsorbent for efficiently removing gaseous benzene series and preparation method and application thereof |
| CN112452355A (en) * | 2020-12-10 | 2021-03-09 | 浙江海洋大学 | Preparation method of carbon material catalyst applied to styrene preparation |
| CN112452355B (en) * | 2020-12-10 | 2023-08-01 | 浙江海洋大学 | Preparation method of carbon material catalyst applied to preparation of styrene |
| CN113231014A (en) * | 2021-04-12 | 2021-08-10 | 东南大学 | Hydrophobic biomass polydopamine composite activated carbon and preparation method thereof |
| CN113368826A (en) * | 2021-07-06 | 2021-09-10 | 江阴市锦绣江南环境发展有限公司 | Adsorbent for heavy metal wastewater treatment and preparation method thereof |
| CN113368826B (en) * | 2021-07-06 | 2023-11-07 | 江阴市锦绣江南环境发展有限公司 | Adsorbent for heavy metal wastewater treatment and preparation method thereof |
| CN117384647A (en) * | 2023-12-11 | 2024-01-12 | 同济大学 | Furillic acid composite nitrogen-doped magnetic carbon submicron sphere and preparation method and application thereof |
| CN117384647B (en) * | 2023-12-11 | 2024-03-22 | 同济大学 | Furillic acid composite nitrogen-doped magnetic carbon submicron sphere and preparation method and application thereof |
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