CN105752980A - Preparation method of composite bio-based porous carbon material - Google Patents
Preparation method of composite bio-based porous carbon material Download PDFInfo
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- CN105752980A CN105752980A CN201610267288.8A CN201610267288A CN105752980A CN 105752980 A CN105752980 A CN 105752980A CN 201610267288 A CN201610267288 A CN 201610267288A CN 105752980 A CN105752980 A CN 105752980A
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- porous carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The invention discloses a preparation method of a composite bio-based porous carbon material, and belongs to the field of porous carbon materials.The method comprises the steps that pigskin collagen is obtained from pigskin, the pigskin collagen is mixed with distiller's grains, peach gum and beet molasses, and yeast powder is added to the mixture for fermentation; a fermented product is subjected to carbonization, and a composite bio-based carbon material crude product is obtained; the composite bio-based carbon material crude product and potassium hydroxide are mixed and put into a tube type resistance furnace, titanium dioxide is introduced and serves as an activating agent for activation, and the composite bio-based porous carbon material is obtained.According to the preparation method of the composite bio-based porous carbon material, the pigskin is utilized and subjected to the processes such as extraction, fermentation, carbonization and activation, rich micropore channels are introduced in the surface of the pigskin, crossed network pore channels are formed, the specific surface area of pores is large, the pore diameter is small, the pores are uniformly distributed, the raw materials are rich, the cost is low, the chemical stability is high, and the composite bio-based porous carbon material can be widely applied in electrodes of supercapacitors.
Description
Technical field
The preparation method that the invention discloses a kind of compound bio base porous carbon materials, belongs to porous carbon materials field.
Background technology
Porous carbon materials is by the highly porous material of extensive concern in carbon nanomaterial family.In recent years, the researcher of material science is actively working to design and develops the novel porous nano material with tunable pore passage structure, the especially research and development of porous carbon materials.Multi-stage porous carbon material section, because having the Electronic Transport of Two Benzene of the pore structure of prosperity, good chemical stability, high specific surface area, superior acid and alkali-resistance and uniqueness, stores and all there is potential using value in the field such as catalyst carrier at electrode material, absorption, separation, sensing, gas.
Generally with coal and Colophonium for the multistage hole Carbon Materials that raw material is prepared, possesses higher thermal conductivity；With high polymer, phenolic resin for multistage hole charcoal prepared by raw material, its thermal conductivity is relatively low.Preparing multistage hole charcoal with biomass for raw material along with the pursuit of environmental protection cleaning technology is created by people in recent years, biomass-based multistage hole charcoal is a kind of novel feature of environmental protection material, has certain dynamogenetic value.
A lot of carbonaceous materials can serve as the presoma of porous charcoal, as a whole, the presoma of porous charcoal may be summarized to be two big classes: the petrochemicals of (1) carbon containing and some macromolecular materials, as: coal, petroleum coke, Colophonium, polyethylene, acrylonitrile, phenolic resin, Carbon fibe etc.；(2) biomass-based carbonaceous material, mainly bamboo and wood, shell, pit, wood machining residues etc., as: sunflower shell, Pericarppium arachidis hypogaeae, orange peel, soybean pod, corn cob, rice husk, coconut husk etc..Along with developing rapidly of global industry, the non-renewable resources such as substantial amounts of coal, oil are constantly consumed, and cause the shortage of resource.Therefore we have to look for a kind of new energy and reduce or substitute the consumption of non-renewable resources.Utilize reproducible biomass to replace day by day exhausted Fossil fuel as carbon source, be the direction of the following whole nation or even global evolution.Owing to biomass are cheap, wide material sources, so adopting biomass as the important component part in raw material porous carbon materials in the future field of porous carbon materials.
Summary of the invention
nullThe technical problem that present invention mainly solves: be mostly to prepare with non-renewable coal and Colophonium for raw material for current conventional porous material with carbon element，There will be hole to subside、Aperture reduces、The phenomenon that porosity and specific surface area reduce，This can be substantially reduced the problem of serviceability of porous carbon materials，The preparation method providing a kind of compound bio base porous carbon materials，The present invention obtains pigskin collagen from Corii Sus domestica，By pigskin collagen and Chinese liquor groove、Resina persicae、Beet molasses mixing adds yeast powder and ferments，Fermented product is carried out carbonization and obtains compound bio base material with carbon element crude product，It is put in tube type resistance furnace with potassium hydroxide mixing，And to pass into titanium dioxide be that activator activates to obtain the base composite porous material with carbon element of compound bio，The present invention utilizes Corii Sus domestica extracting、Fermentation、Carbonization、After the techniques such as activation，It is made to introduce abundant micropore canals on surface，Form the network duct intersected，The specific surface area in hole is big、Aperture is less，Pore size distribution is uniform，And abundant raw material，It it is renewable raw materials，With low cost、Chemical stability is high，Can be widely used in the preparation of the electrode of ultracapacitor.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
1.(1) weigh 1～2kg Corii Sus domestica dissecting knife strike off fat deposit and be cut into the fritter of 5mm × 5mm, put into and iron pan adds distilled water until submergence Corii Sus domestica fritter, it is warming up to 90～100 DEG C, then in pot, adds the sodium bicarbonate powder of Corii Sus domestica fritter quality 10%, insulated and stirred defat 10～15min；
2.(2) defat filters moisture after terminating, with deionized water rinsing Corii Sus domestica fritter to neutral, put it into sonic oscillation instrument, add dehydrated alcohol submergence, after 200～300W power ultrasonic oscillation treatment 30～40min, filter and filtering residue is moved into baking oven, be dried overnight at 60～80 DEG C, obtain pigskin collagen block；
Impurity is removed with water rinsing after 3.(3) weighing 400～500g distillers ' grains and 200～300g Resina persicae mix homogeneously, mixture vacuum drier after washing is moved in ceramic pot after drying, add 500～600g pigskin collagen block obtained above and 100～200mL beet molasses, stir by stirring rod, obtain mixing purees；
4.(4) take the yeast powder of above-mentioned mixing purees gross mass 1～2%, mix well prepared yeast mixture with the warm water of its volume 2～3 times 25～30 DEG C, yeast mixture is poured in above-mentioned ceramic pot, after stirring at 40～45 DEG C heat-preservation fermentation 3～5h；
5.(5) after fermentation ends, fermented product is moved in retort, with the speed of 100mL/min to stove passing into after nitrogen purges 20～30min, it is heated to 600～700 DEG C, insulation carbonization 2～3h, it is cooled to after room temperature until it, carbonizing production is put into and jet mill is pulverized and crosses 100 mesh standard sieves, obtain compound bio base material with carbon element crude product；
Put in tube type resistance furnace after 6.(6) compound bio base material with carbon element crude product obtained above and potassium hydroxide powder being mixed for 1:3 in mass ratio, pass into nitrogen displacement and come out of the stove after interior all air, it is warming up in 800～900 DEG C of backward stoves with 10 DEG C/min rate program and passes into carbon dioxide as activator using 60～80mL/min speed, after insulation activation processing 1～2h, namely discharging obtains compound bio base porous carbon materials.
The application process of the present invention: it is 1126.2～1163.5m that the present invention prepares the specific surface area of compound bio base porous carbon materials2/ g, pore volume is 0.34～0.49cm3/ g, by bio-based porous carbon materials: acetylene black: politef=80:10:10 (mass ratio), make half-dried slurry, it is pressed in nickel foam (15MPa), prepare into electrode, and its chemical property is tested: when electric current is 0.5A/g, test voltage ranges for 1.0～1.5V, than electric capacity up to 288.9～325.9F/g, 10000 later electric capacity of cycle charge-discharge are almost without loss.
The invention has the beneficial effects as follows:
(1) present invention utilizes Corii Sus domestica after the techniques such as extraction, fermentation, carbonization, activation so that it is introduces abundant micropore canals on surface, forms the network duct intersected, and specific surface area is big, aperture is less, is evenly distributed；
(2) present invention utilizes Corii Sus domestica for biomass material, abundance, with low cost, chemical stability is high.
Detailed description of the invention
First weigh 1～2kg Corii Sus domestica dissecting knife strike off fat deposit and be cut into the fritter of 5mm × 5mm, put into and iron pan adds distilled water until submergence Corii Sus domestica fritter, it is warming up to 90～100 DEG C, then in pot, adds the sodium bicarbonate powder of Corii Sus domestica fritter quality 10%, insulated and stirred defat 10～15min；Defat filters moisture after terminating, and with deionized water rinsing Corii Sus domestica fritter to neutral, puts it into sonic oscillation instrument, add dehydrated alcohol submergence, after 200～300W power ultrasonic oscillation treatment 30～40min, filter and filtering residue is moved into baking oven, it is dried overnight at 60～80 DEG C, obtains pigskin collagen block；Impurity is removed with water rinsing after weighing 400～500g distillers ' grains and 200～300g Resina persicae mix homogeneously, mixture vacuum drier after washing is moved in ceramic pot after drying, add 500～600g pigskin collagen block obtained above and 100～200mL beet molasses, stir by stirring rod, obtain mixing purees；Take the yeast powder of above-mentioned mixing purees gross mass 1～2%, mix well prepared yeast mixture with the warm water of its volume 2～3 times 25～30 DEG C, yeast mixture is poured in above-mentioned ceramic pot, after stirring at 40～45 DEG C heat-preservation fermentation 3～5h；After fermentation ends, fermented product is moved in retort, with the speed of 100mL/min to stove passing into after nitrogen purges 20～30min, it is heated to 600～700 DEG C, insulation carbonization 2～3h, it is cooled to after room temperature until it, carbonizing production is put into and jet mill is pulverized and crosses 100 mesh standard sieves, obtain compound bio base material with carbon element crude product；Put in tube type resistance furnace after compound bio base material with carbon element crude product obtained above and potassium hydroxide powder are mixed for 1:3 in mass ratio, pass into nitrogen displacement and come out of the stove after interior all air, it is warming up in 800～900 DEG C of backward stoves with 10 DEG C/min rate program and passes into carbon dioxide as activator using 60～80mL/min speed, after insulation activation processing 1～2h, namely discharging obtains compound bio base porous carbon materials.
Example 1
8. first weigh 1kg Corii Sus domestica dissecting knife strike off fat deposit and be cut into the fritter of 5mm × 5mm, put into and iron pan adds distilled water until submergence Corii Sus domestica fritter, it is warming up to 90 DEG C, then in pot, adds the sodium bicarbonate powder of Corii Sus domestica fritter quality 10%, insulated and stirred defat 10min；Defat filters moisture after terminating, and with deionized water rinsing Corii Sus domestica fritter to neutral, puts it into sonic oscillation instrument, add dehydrated alcohol submergence, after 200W power ultrasonic oscillation treatment 30min, filter and filtering residue is moved into baking oven, it is dried overnight at 60 DEG C, obtains pigskin collagen block；Impurity is removed with water rinsing after weighing 400g distillers ' grains and 200g Resina persicae mix homogeneously, mixture vacuum drier after washing is moved in ceramic pot after drying, add 500g pigskin collagen block obtained above and 100mL beet molasses, stir by stirring rod, obtain mixing purees；Take the yeast powder of above-mentioned mixing purees gross mass 1%, mix well prepared yeast mixture with the warm water of its volume 2 times 25 DEG C, yeast mixture is poured in above-mentioned ceramic pot, after stirring at 40 DEG C heat-preservation fermentation 3h；After fermentation ends, fermented product is moved in retort, with the speed of 100mL/min to stove passing into after nitrogen purges 20min, it is heated to 600 DEG C, insulation carbonization 2h, it is cooled to after room temperature until it, carbonizing production is put into and jet mill is pulverized and crosses 100 mesh standard sieves, obtain compound bio base material with carbon element crude product；Put in tube type resistance furnace after compound bio base material with carbon element crude product obtained above and potassium hydroxide powder are mixed for 1:3 in mass ratio, pass into nitrogen displacement and come out of the stove after interior all air, it is warming up in 800 DEG C of backward stoves with 10 DEG C/min rate program and passes into carbon dioxide as activator using 60mL/min speed, after insulation activation processing 1h, namely discharging obtains compound bio base porous carbon materials.
It is 1126.2m that the present invention prepares the specific surface area of compound bio base porous carbon materials2/ g, pore volume is 0.34cm3/ g, by bio-based porous carbon materials: acetylene black: politef=80:10:10 (mass ratio), make half-dried slurry, it is pressed in nickel foam (15MPa), prepare into electrode, and its chemical property is tested: when electric current is 0.5A/g, test voltage ranges for 1.0V, than electric capacity up to 288.9F/g, 10000 later electric capacity of cycle charge-discharge are almost without loss.
Example 2
9. first weigh 1.5kg Corii Sus domestica dissecting knife strike off fat deposit and be cut into the fritter of 5mm × 5mm, put into and iron pan adds distilled water until submergence Corii Sus domestica fritter, it is warming up to 95 DEG C, then in pot, adds the sodium bicarbonate powder of Corii Sus domestica fritter quality 10%, insulated and stirred defat 13min；Defat filters moisture after terminating, and with deionized water rinsing Corii Sus domestica fritter to neutral, puts it into sonic oscillation instrument, add dehydrated alcohol submergence, after 250W power ultrasonic oscillation treatment 35min, filter and filtering residue is moved into baking oven, it is dried overnight at 70 DEG C, obtains pigskin collagen block；Impurity is removed with water rinsing after weighing 450g distillers ' grains and 250g Resina persicae mix homogeneously, mixture vacuum drier after washing is moved in ceramic pot after drying, add 550g pigskin collagen block obtained above and 150mL beet molasses, stir by stirring rod, obtain mixing purees；Take the yeast powder of above-mentioned mixing purees gross mass 1%, mix well prepared yeast mixture with the warm water of its volume 2.5 times 28 DEG C, yeast mixture is poured in above-mentioned ceramic pot, after stirring at 43 DEG C heat-preservation fermentation 4h；After fermentation ends, fermented product is moved in retort, with the speed of 100mL/min to stove passing into after nitrogen purges 25min, it is heated to 650 DEG C, insulation carbonization 2.5h, it is cooled to after room temperature until it, carbonizing production is put into and jet mill is pulverized and crosses 100 mesh standard sieves, obtain compound bio base material with carbon element crude product；Put in tube type resistance furnace after compound bio base material with carbon element crude product obtained above and potassium hydroxide powder are mixed for 1:3 in mass ratio, pass into nitrogen displacement and come out of the stove after interior all air, it is warming up in 850 DEG C of backward stoves with 10 DEG C/min rate program and passes into carbon dioxide as activator using 70mL/min speed, after insulation activation processing 1.5h, namely discharging obtains compound bio base porous carbon materials.
It is 1145.5m that the present invention prepares the specific surface area of compound bio base porous carbon materials2/ g, pore volume is 0.45cm3/ g, by bio-based porous carbon materials: acetylene black: politef=80:10:10 (mass ratio), make half-dried slurry, it is pressed in nickel foam (15MPa), prepare into electrode, and its chemical property is tested: when electric current is 0.5A/g, test voltage ranges for 1.2V, than electric capacity up to 304.7F/g, 10000 later electric capacity of cycle charge-discharge are almost without loss.
Example 3
10. first weigh 2kg Corii Sus domestica dissecting knife strike off fat deposit and be cut into the fritter of 5mm × 5mm, put into and iron pan adds distilled water until submergence Corii Sus domestica fritter, it is warming up to 100 DEG C, then in pot, adds the sodium bicarbonate powder of Corii Sus domestica fritter quality 10%, insulated and stirred defat 15min；Defat filters moisture after terminating, and with deionized water rinsing Corii Sus domestica fritter to neutral, puts it into sonic oscillation instrument, add dehydrated alcohol submergence, after 300W power ultrasonic oscillation treatment 40min, filter and filtering residue is moved into baking oven, it is dried overnight at 80 DEG C, obtains pigskin collagen block；Impurity is removed with water rinsing after weighing 500g distillers ' grains and 300g Resina persicae mix homogeneously, mixture vacuum drier after washing is moved in ceramic pot after drying, add 600g pigskin collagen block obtained above and 100～200mL beet molasses, stir by stirring rod, obtain mixing purees；Take the yeast powder of above-mentioned mixing purees gross mass 2%, mix well prepared yeast mixture with the warm water of its volume 3 times 30 DEG C, yeast mixture is poured in above-mentioned ceramic pot, after stirring at 45 DEG C heat-preservation fermentation 5h；After fermentation ends, fermented product is moved in retort, with the speed of 100mL/min to stove passing into after nitrogen purges 30min, it is heated to 700 DEG C, insulation carbonization 3h, it is cooled to after room temperature until it, carbonizing production is put into and jet mill is pulverized and crosses 100 mesh standard sieves, obtain compound bio base material with carbon element crude product；Put in tube type resistance furnace after compound bio base material with carbon element crude product obtained above and potassium hydroxide powder are mixed for 1:3 in mass ratio, pass into nitrogen displacement and come out of the stove after interior all air, it is warming up in 900 DEG C of backward stoves with 10 DEG C/min rate program and passes into carbon dioxide as activator using 80mL/min speed, after insulation activation processing 2h, namely discharging obtains compound bio base porous carbon materials.
It is 1163.5m that the present invention prepares the specific surface area of compound bio base porous carbon materials2/ g, pore volume is 0.49cm3/ g, by bio-based porous carbon materials: acetylene black: politef=80:10:10 (mass ratio), make half-dried slurry, it is pressed in nickel foam (15MPa), prepare into electrode, and its chemical property is tested: when electric current is 0.5A/g, test voltage ranges for 1.5V, than electric capacity up to 325.9F/g, 10000 later electric capacity of cycle charge-discharge are almost without loss.
Claims (1)
1. the preparation method of a compound bio base porous carbon materials, it is characterised in that concrete preparation process is:
(1) weigh 1～2kg Corii Sus domestica dissecting knife strike off fat deposit and be cut into the fritter of 5mm × 5mm, put into and iron pan adds distilled water until submergence Corii Sus domestica fritter, it is warming up to 90～100 DEG C, then in pot, adds the sodium bicarbonate powder of Corii Sus domestica fritter quality 10%, insulated and stirred defat 10～15min；
(2) defat filters moisture after terminating, with deionized water rinsing Corii Sus domestica fritter to neutral, put it into sonic oscillation instrument, add dehydrated alcohol submergence, after 200～300W power ultrasonic oscillation treatment 30～40min, filter and filtering residue is moved into baking oven, be dried overnight at 60～80 DEG C, obtain pigskin collagen block；
(3) impurity is removed with water rinsing after weighing 400～500g distillers ' grains and 200～300g Resina persicae mix homogeneously, mixture vacuum drier after washing is moved in ceramic pot after drying, add 500～600g pigskin collagen block obtained above and 100～200mL beet molasses, stir by stirring rod, obtain mixing purees；
(4) take the yeast powder of above-mentioned mixing purees gross mass 1～2%, mix well prepared yeast mixture with the warm water of its volume 2～3 times 25～30 DEG C, yeast mixture is poured in above-mentioned ceramic pot, after stirring at 40～45 DEG C heat-preservation fermentation 3～5h；
(5) after fermentation ends, fermented product is moved in retort, with the speed of 100mL/min to stove passing into after nitrogen purges 20～30min, it is heated to 600～700 DEG C, insulation carbonization 2～3h, it is cooled to after room temperature until it, carbonizing production is put into and jet mill is pulverized and crosses 100 mesh standard sieves, obtain compound bio base material with carbon element crude product；
(6) put in tube type resistance furnace after compound bio base material with carbon element crude product obtained above and potassium hydroxide powder being mixed for 1:3 in mass ratio, pass into nitrogen displacement and come out of the stove after interior all air, it is warming up in 800～900 DEG C of backward stoves with 10 DEG C/min rate program and passes into carbon dioxide as activator using 60～80mL/min speed, after insulation activation processing 1～2h, namely discharging obtains compound bio base porous carbon materials.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629723A (en) * | 2016-12-30 | 2017-05-10 | 扬州大学 | Biomass-based N, S and P-containing co-doped porous carbon and application thereof |
| CN107022283A (en) * | 2017-03-28 | 2017-08-08 | 常州大学 | A kind of preparation method of ultraviolet light curing cathodic electrophoretic coating compound resin |
| CN108483443A (en) * | 2018-03-30 | 2018-09-04 | 江苏新亿源环保科技有限公司 | A kind of preparation method of high absorption multiporous biological matter based foam carbon |
| CN108816193A (en) * | 2018-06-14 | 2018-11-16 | 华南理工大学 | One kind having superelevation ultramicropore molasses base carbon material and the preparation method and application thereof |
| CN110436929A (en) * | 2017-06-07 | 2019-11-12 | 吴彬 | A kind of silicon carbide ceramics |
| CN111268677A (en) * | 2020-01-20 | 2020-06-12 | 辽宁大学 | Preparation method and application of novel lithium ion battery negative electrode material carbonized grape seed |
| CN113314352A (en) * | 2021-06-09 | 2021-08-27 | 东莞理工学院 | Method for preparing high-performance supercapacitor spore carbon electrode |
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2016
- 2016-04-27 CN CN201610267288.8A patent/CN105752980A/en not_active Withdrawn
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629723A (en) * | 2016-12-30 | 2017-05-10 | 扬州大学 | Biomass-based N, S and P-containing co-doped porous carbon and application thereof |
| CN107022283A (en) * | 2017-03-28 | 2017-08-08 | 常州大学 | A kind of preparation method of ultraviolet light curing cathodic electrophoretic coating compound resin |
| CN110436929A (en) * | 2017-06-07 | 2019-11-12 | 吴彬 | A kind of silicon carbide ceramics |
| CN108483443A (en) * | 2018-03-30 | 2018-09-04 | 江苏新亿源环保科技有限公司 | A kind of preparation method of high absorption multiporous biological matter based foam carbon |
| CN108816193A (en) * | 2018-06-14 | 2018-11-16 | 华南理工大学 | One kind having superelevation ultramicropore molasses base carbon material and the preparation method and application thereof |
| CN108816193B (en) * | 2018-06-14 | 2021-02-19 | 华南理工大学 | Molasses-based carbon material with ultrahigh ultramicropore and preparation method and application thereof |
| CN111268677A (en) * | 2020-01-20 | 2020-06-12 | 辽宁大学 | Preparation method and application of novel lithium ion battery negative electrode material carbonized grape seed |
| CN113314352A (en) * | 2021-06-09 | 2021-08-27 | 东莞理工学院 | Method for preparing high-performance supercapacitor spore carbon electrode |
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Application publication date: 20160713 |