CN104843668A - Method for preparing nitrogen doped porous carbon material by using biologic proteins - Google Patents
Method for preparing nitrogen doped porous carbon material by using biologic proteins Download PDFInfo
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Abstract
The invention provides a method for preparing a nitrogen doped porous carbon material by using biologic proteins. The method mainly comprises the following steps: 1, mixing the biologic proteins with an acid or alkali or salt solution; 2, carbonizing the above obtained dried mixture under the protection of inert gas; and 3, carrying out distilled water addition, pumping filtration and washing until the pH value is 6.4-7, and drying to obtain solid powder which is the nitrogen doped porous carbon material. The widely and easily available biologic proteins are adopted as raw materials, and the raw materials comprise silk fibroin, albumen and soybean proteins, so the method has the advantages of simple operating technology, convenient control, cleanness, environmental protection, and easy industrial realization. The prepared nitrogen doped porous carbon material has the advantages of large specific surface area, low ash content and good conductivity. The nitrogen doped porous carbon material can be used in lithium ion batteries, lithium sulfur batteries, super capacitors and other electrode materials, and fields of carbon dioxide capture, hydrogen storage, catalyst carriers, active carbon adsorbents and biologic applications.
Description
Technical field
The invention provides a kind of method that bioprotein prepares the porous carbon material of nitrating, belong to porous carbon material preparation field.
Background technology
Porous charcoal mainly with various shell (Exocarpium cocois (Cocos nucifera L), apricot shell, nut-shell etc.), the contour carbonaceous material of bamboo wood chip, coal for raw material, the Carbon Materials of the vesicular structure of the advantages such as the adsorptivity ability had obtained by pyrolysis is strong, pore passage structure is complicated, unreactiveness is good, be widely used in, 1. Gas Phase Adsorption, such as can be used as methane, the storage of hydrogen and Sweet natural gas; 2. the electrode materials of energy storage device, the positive electrode material of such as lithium-sulfur cell, electrode material for super capacitor, lithium ion battery negative material, lithium air battery positive electrode material etc.; 3. as the application of catalyzer and support of the catalyst, the such as field such as unpolarizing of oxygen in the hydrolysis of ester class, flue gas desulfurization (FGD), battery, especially redox reaction.Wherein high surface area activated carbon, provides sound response center and load; 4. clinical treatment application, as cancer therapy, blood is evolved, oral urgent toxicide etc.; 5. liquid phase adsorption, such as, organic pollutant and metal biosorption etc.Porous carbon material has become the product that people live and the national economic development is indispensable.Although common porous carbon be widely used in every field, because its structure and composition qualities determine that its application power is limited, still govern the application widely of carbon material, and in the process of preparation easy contaminate environment.Bioprotein, also claims biological activity protein, and being the general name of the different peptide classes of linear, the ring structure from dipeptides to complexity that in protein, 25 natural amino acids are formed with difference composition and arrangement mode, is the multi-functional compounds coming from protein.The present invention is with the bioprotein be extensively easy to get for raw material, and raw material comprises silk fibroin, albumen, soybean protein etc.In what is more important bioprotein, the content of nitrogen element is about 16%, it is good nitrogenous source, not only aboundresources, and it is cheap and renewable, the porous carbon material of nitrating is as the porous material of functionalization, specific surface area, pore size distribution have important impact to performance, and current China exists the problems such as Activated Carbon Production lacks pore size distribution control measures and the content of nitrogen element is low, specificity application is not strong.While the present invention has the porous carbon material preparing high-specific surface area nitrating, orientation regulation and control are carried out to its microtexture structure, contribute to improving further and expand the professional application of porous material, and design technology process is simple, clean environment firendly, be easy to industrialization realization.
Summary of the invention
The present invention is directed to the deficiency that existing porous carbon preparation method for material exists, provide a kind of with bioprotein be raw material prepare the adjustable preparation method of high-specific surface area, the content of nitrogen element and pore size distribution.
The object of the invention is to be achieved through the following technical solutions.
Bioprotein prepares a method for the porous carbon material of nitrating, comprises the steps:
Step one: bioprotein is mixed with the one in acid, alkali, saline solution under field conditions (factors) or under low temperature;
Step 2: by 350 DEG C ~ 1900 DEG C carbonizations under protection of inert gas of dried mixture.One is in microwave device, microwave radiation under the power of 300 ~ 2500W, 2 ~ 40 minutes, and one is activate 10 ~ 800 minutes in carbide furnace;
Step 3: be dry after 6.4 ~ 7 with adding distil water filtering and washing to pH value, prepares nitrating porous carbon material.
The method preparing the porous carbon material of nitrating as described in specification sheets step one, the presoma wherein preparing the porous carbon material of nitrating is bioprotein, or containing bioprotein, or with the product after bioprotein process.
The step one prepared in the method for the porous carbon material of nitrating as used in the description, the selection of the solution wherein mixed, comprises acidic solution such as, as phosphoric acid hydrogen ammonia, phosphoric acid, ammonium di-hydrogen phosphate etc.
The step one prepared in the method for the porous carbon material of nitrating as used in the description, the selection of the solution wherein mixed, comprises basic solution such as, as potassium hydroxide solution, solution of potassium carbonate, sodium hydroxide solution, sodium carbonate solution, ammonia soln etc.
The step one prepared in the method for the porous carbon material of nitrating as used in the description, the selection of the solution wherein mixed, comprises saline solution such as, as calcium chloride, zinc chloride, magnesium chloride, iron(ic) chloride etc.
Carbonization described in step 2 (bioprotein) mixes with different substances (solution), when wherein material (solution) is acid, be that the acid being greater than 0.1% is flooded 1 ~ 100 hour at temperature 0 DEG C ~ 100 DEG C by its massfraction, described acid is the reagent of all acidity, and namely the pH value of the aqueous solution of reagent is less than 7, as phosphoric acid, sulfuric acid, nitric acid, phosphoric acid hydrogen ammonia, ammonium di-hydrogen phosphate etc.
Carbonization described in step 2 (bioprotein) mixes with different substances (solution), when wherein material (solution) is alkalescence, described alkali is the reagent of all alkalescence, namely the pH value of the aqueous solution of reagent is less than 7, or or solid matter be dissolved in solvent after pH value be greater than 7.As potassium hydroxide solution, solution of potassium carbonate, sodium hydroxide solution, sodium carbonate solution, ammonia soln etc.
Carbonization described in step 2 (bioprotein) mixes with different substances (solution), when wherein material (solution) is for salt, and described salt, as magnesium chloride, zinc chloride, iron(ic) chloride etc. and their solution.
The method preparing the porous carbon material of nitrating as used in the description, the porous carbon material of the nitrating wherein prepared is also included within direct carbonization bioprotein under atmosphere of inert gases.
The method preparing the porous carbon material of nitrating as used in the description, the porous carbon material of the nitrating wherein prepared is also included within direct carbonization bioprotein under the atmosphere such as water vapour or carbonic acid gas.
Beneficial effect
1, the present invention is a kind of method preparing nitrating porous carbon material, and design technology process is simple, clean environment firendly, conveniently controls, is easy to industrialization realization;
2, the invention provides a kind of aperture of preparing and can be in harmonious proportion the nitrating porous carbon material of high-specific surface area;
3, the material prepared by the present invention can be used to the electrode materialss such as the empty sulphur battery of lithium, lithium ion battery, lithium-sulfur cell, ultracapacitor, catches carbonic acid gas, storage methane gas, storage hydrogen, the sorbent material of environmental pollutant, the various field such as support of the catalyst.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of preparation method of the present invention;
Fig. 2 is scanning electron microscope (SEM) figure and transmission electron microscope (TEM) figure of the porous carbon material of nitrating prepared in embodiment 1;
Fig. 3 is the nitrogen adsorption desorption curve of the porous carbon material of the nitrating executing example preparation, pore size distribution curve figure.
Embodiment
Below in conjunction with drawings and Examples, the present invention is elaborated.
Embodiment 1
Utilize nitrating porous carbon material prepared by preparation system of the present invention.
Step one: silk fibroin is mixed with the one in the material of acidity or solution under field conditions (factors) or under low temperature;
Step 2: by the 850 DEG C of carbonizations under protection of inert gas of dried mixture.
Step 3: be dry after 6.4 ~ 7 with adding distil water filtering and washing to pH value, prepares nitrating porous carbon material.
Embodiment 2
Utilize nitrating porous carbon material prepared by preparation system of the present invention.
Step one: soybean protein is mixed with the one in the material of acidity or solution under field conditions (factors) or under low temperature;
Step 2: by dried mixture under protection of inert gas, in microwave device, microwave radiation 40 minutes under the power of 1000W.
Step 3: be dry after 6.4 ~ 7 with adding distil water filtering and washing to pH value, prepares nitrating porous carbon material.
Embodiment 3
Utilize nitrating porous carbon material prepared by preparation system of the present invention.
Step one: silk fibroin is mixed with the one in the material of acidity or solution under field conditions (factors) or under low temperature;
Step 2: by dried mixture under protection of inert gas, carbonization 100 minutes in tubular type stove.
Step 3: be dry after 6.4 ~ 7 with adding distil water filtering and washing to pH value, prepares nitrating porous carbon material.
Embodiment 4
Utilize nitrating porous carbon material prepared by preparation system of the present invention.
Step one: albumen is mixed with the one in the material of alkalescence or solution under field conditions (factors) or under low temperature;
Step 2: by the 880 DEG C of carbonizations under protection of inert gas of dried mixture.
Step 3: first ultrasonic with adding dilute hydrochloric acid, then be 6.4 ~ 7 rear dryings with distilled water filtering and washing to pH value, prepare nitrating porous carbon material.
Embodiment 5
Utilize nitrating porous carbon material prepared by preparation system of the present invention.
Step one: silk fibroin is mixed with the one in the material of acidity or solution under field conditions (factors) or under low temperature;
Step 2: by dried mixture under protection of inert gas, in microwave device, microwave radiation 50 minutes under the power of 1000W.
Step 3: first ultrasonic with adding dilute hydrochloric acid, then be 6.4 ~ 7 rear dryings with distilled water filtering and washing to pH value, prepare nitrating porous carbon material.
Embodiment 6
Utilize nitrating porous carbon material prepared by preparation system of the present invention.
Step one: silk fibroin is mixed with the one in the material of acidity or solution under field conditions (factors) or under low temperature;
Step 2: by dried mixture under protection of inert gas, carbonization 100 minutes in tubular type stove.
Step 3: first ultrasonic with adding dilute hydrochloric acid, then be 6.4 ~ 7 rear dryings with distilled water filtering and washing to pH value, prepare nitrating porous carbon material.
Embodiment 7
Utilize nitrating porous carbon material prepared by preparation system of the present invention.
Step one: albumen is mixed with the one in the material of salt or solution under field conditions (factors) or under low temperature;
Step 2: by the 820 DEG C of carbonizations under protection of inert gas of dried mixture.
Step 3: first ultrasonic with adding dilute hydrochloric acid, then be 6.4 ~ 7 rear dryings with distilled water filtering and washing to pH value, prepare nitrating porous carbon material.
Embodiment 8
Utilize nitrating porous carbon material prepared by preparation system of the present invention.
Step one: soybean protein is mixed with the one in the material of salt or solution under field conditions (factors) or under low temperature;
Step 2: by dried mixture under protection of inert gas, in microwave device, microwave radiation 200 minutes under the power of 500W.
Step 3: first ultrasonic with adding dilute hydrochloric acid, then be 6.4 ~ 7 rear dryings with distilled water filtering and washing to pH value, prepare nitrating porous carbon material.
Embodiment 9
Utilize nitrating porous carbon material prepared by preparation system of the present invention.
Step one: silk fibroin is mixed with the one in the material of salt or solution under field conditions (factors) or under low temperature;
Step 2: by dried mixture under protection of inert gas, carbonization 180 minutes in tubular type stove.
Step 3: first ultrasonic with adding dilute hydrochloric acid, then be 6.4 ~ 7 rear dryings with distilled water filtering and washing to pH value, prepare nitrating porous carbon material.
Embodiment 10
Utilize nitrating porous carbon material prepared by preparation system of the present invention.
Step one: by albumen directly 920 DEG C of carbonizations under protection of inert gas, prepare nitrating porous carbon material.
Embodiment 11
Utilize nitrating porous carbon material prepared by preparation system of the present invention.
Step one: by soybean protein directly 1100 DEG C of carbonizations under protection of inert gas, prepare nitrating porous carbon material.
Embodiment 12
Utilize nitrating porous carbon material prepared by preparation system of the present invention.
Step one: by silk fibroin directly in CO 2 gas-shielded lower 950 DEG C of carbonizations, prepare nitrating porous carbon material.
Embodiment 13
Utilize nitrating porous carbon material prepared by preparation system of the present invention.
Step one: by bioprotein directly in CO 2 gas-shielded lower 1050 DEG C of carbonizations, prepare nitrating porous carbon material.
Embodiment 14
Utilize nitrating porous carbon material prepared by preparation system of the present invention.
Step one: by albumen directly 850 DEG C of carbonization-activations under water vapor gas protection, prepare nitrating porous carbon material.
Embodiment 15
Utilize nitrating porous carbon material prepared by preparation system of the present invention.
Step one: by soybean protein directly at CO 2 gas-shielded lower 950 DEG C of carbonization-activations, prepare nitrating porous carbon material.
Above-described specific descriptions; the object of inventing, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; the protection domain be not intended to limit the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. prepare a method for the porous carbon material of nitrating with bioprotein, the method comprises:
Step one: bioprotein is mixed with the one in acid, alkali, saline solution under field conditions (factors) or under low temperature;
Step 2: by 350 DEG C ~ 1900 DEG C carbonizations under protection of inert gas of dried mixture.One is in microwave device, microwave radiation under the power of 300 ~ 2500W, 2 ~ 40 minutes, and one is activate 10 ~ 800 minutes in carbide furnace;
Step 3: be dry after 6.4 ~ 7 with adding distil water filtering and washing to pH value, prepares nitrating porous carbon material.
2. prepare the method for the porous carbon material of nitrating as claimed in claim 1, the presoma wherein preparing the porous carbon material of nitrating is bioprotein, or containing bioprotein, or with the product after bioprotein process.
3. prepare the method for the porous carbon material of nitrating as claimed in claim 1, the presoma wherein preparing the porous carbon material of nitrating is bioprotein, and bioprotein raw material comprises silk fibroin, albumen, soybean protein etc., different kind organism albumen.
4. prepare the method for the porous carbon material of nitrating as claimed in claim 1, the selection of the solution wherein mixed, comprise acidic solution such as, as phosphoric acid hydrogen ammonia, phosphoric acid, ammonium di-hydrogen phosphate etc.
5. prepare the method for the porous carbon material of nitrating as claimed in claim 1, the selection of the solution wherein mixed, comprise basic solution such as, as potassium hydroxide solution, solution of potassium carbonate, sodium hydroxide solution, sodium carbonate solution, ammonia soln etc.
6. prepare the method for the porous carbon material of nitrating as claimed in claim 1, the selection of the solution wherein mixed, comprise saline solution such as, as calcium chloride, zinc chloride, magnesium chloride, iron(ic) chloride etc.
7. prepare the method for the porous carbon material of nitrating as claimed in claim 1, the porous carbon material of the nitrating wherein prepared also comprises direct carbonization bioprotein.
8. prepare the method for the porous carbon material of nitrating as claimed in claim 1, the porous carbon material of the nitrating wherein prepared also comprises direct carbonization activation bioprotein, such as, activate by physically activated method, wherein activator is as water vapour, carbonic acid gas, air, hydrogen peroxide etc.
9. prepare the method for the porous carbon material of nitrating as claimed in claim 1, wherein carbonization or activation heat-processed in, both can use and can heat stove or pyroreaction still, also can use microwave device, carry out microwave radiation heating.
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| CN105336930A (en) * | 2015-10-16 | 2016-02-17 | 浙江理工大学 | Nitrogen-enriched carbon based/sulfur composite cathode material used for lithium sulphur batteries, and preparation method thereof |
| CN106006636A (en) * | 2016-05-19 | 2016-10-12 | 中国科学院青岛生物能源与过程研究所 | Biomass-based nitrogen-doped porous carbon material, and preparation method and application thereof |
| CN106744858A (en) * | 2017-01-16 | 2017-05-31 | 深圳大学 | A kind of three-dimensional grapheme and preparation method and application |
| CN106744803A (en) * | 2017-01-23 | 2017-05-31 | 深圳大学 | A kind of method and porous carbon for preparing porous carbon |
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| CN107697914A (en) * | 2017-08-22 | 2018-02-16 | 河南师范大学 | A kind of method for preparing nitrogen-doped porous carbon material |
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| CN109081339A (en) * | 2018-09-19 | 2018-12-25 | 四川大学 | A kind of novel nitrogen-dopped activated carbon for greenhouse gases trapping |
| CN109133029A (en) * | 2018-09-07 | 2019-01-04 | 江苏超电新能源科技发展有限公司 | A kind of preparation method of lithium ion battery negative material and its lithium ion battery of preparation |
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| CN112941552A (en) * | 2021-01-27 | 2021-06-11 | 云南电网有限责任公司电力科学研究院 | Porous carbon-supported ruthenium catalyst and preparation method thereof |
| CN114388737A (en) * | 2021-12-24 | 2022-04-22 | 西安理工大学 | Self-supporting electrode, preparation method thereof and lithium-sulfur battery |
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| CN114388737A (en) * | 2021-12-24 | 2022-04-22 | 西安理工大学 | Self-supporting electrode, preparation method thereof and lithium-sulfur battery |
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