CN109956460A - Preparation method with tridimensional network coal base grading-hole charcoal-aero gel - Google Patents
Preparation method with tridimensional network coal base grading-hole charcoal-aero gel Download PDFInfo
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- CN109956460A CN109956460A CN201910178612.2A CN201910178612A CN109956460A CN 109956460 A CN109956460 A CN 109956460A CN 201910178612 A CN201910178612 A CN 201910178612A CN 109956460 A CN109956460 A CN 109956460A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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Abstract
The present invention relates to a kind of preparations with tridimensional network coal base grading-hole charcoal-aero gel.The aeroge is with the raw coal of nitration mixture oxidation processes (oxidized coal) for raw material, polyvinyl alcohol is as crosslinking agent and pore creating material, potassium hydroxide is added and is adjusted to solution as neutrality, xerogel is obtained by aging, freeze-drying process, xerogel is passed through into high temperature cabonization again, it is different with polyvinyl alcohol degree of decomposition due to oxidized coal and generate classifying porous during high temperature cabonization, and then the coal base grading-hole charcoal-aero gel with tridimensional network is made.Preparation method includes: the preparation with tridimensional network coal base grading-hole charcoal-aero gel.Synthesis process of the present invention is raw material with Xinjiang Heishan coal, resourceful, and cheap, and preparation method is simpler, and there is tridimensional network coal base grading-hole charcoal-aero gel to be expected to be applied to the fields such as supercapacitor for preparation.
Description
What this patent was related to is the preparation method with tridimensional network coal base grading-hole charcoal-aero gel.
Background technique
Supercapacitor, also referred to as electrochemical capacitor are a kind of new between traditional capacitor and secondary cell
The energy storage device of type has the characteristics that efficiency for charge-discharge is high, power density is high, has extended cycle life, is widely used in work
Industry, military, the fields such as communications and transportation.So design structure is reasonable, the high electrode material of specific surface area is to realize that high-performance is super
The key of capacitor.Currently, the highest super capacitor material of commercialization degree is carbon-based material.And charcoal-aero gel, as one
The novel carbon material of kind, has light weight, the advantages such as large specific surface area, pore volume is big, and thermal conductivity is low.In the energy, environmental protection, building
And the fields such as space flight and aviation have broad application prospects.
The research of graphene aerogel and be prepared into a current research hotspot, but graphene aerogel there is
Cost of manufacture is high, and the source of raw material is less, and preparation process is more complex and limits and commercially produces.Therefore, we select coal
Charcoal-aero gel is prepared as carbon source, advantage is as follows: firstly, coal based gas gel utilizes Xinjiang coal resources abundant, price
It is cheap；Secondly, coal-based carbon aeroge preparation process is simple, the cost of charcoal-aero gel can be substantially reduced, to be coal-based carbon airsetting
The large scale preparation of glue, which provides, a kind of may and be expected to be applied to the fields such as supercapacitor.
Summary of the invention
Technical problem to be solved by the invention is to provide one kind to have tridimensional network coal base grading-hole charcoal-aero gel
Preparation method, preparing for this method is simple, at low cost, and the coal base grading-hole charcoal airsetting with tridimensional network is prepared
Glue.
Coal base grading-hole charcoal-aero gel provided by the present invention, preparing raw material includes: coal, the concentrated sulfuric acid, nitric acid, hydroxide
Potassium, polyvinyl alcohol.
Coal base grading-hole charcoal-aero gel provided by the present invention, preparation process include: to be handled with nitration mixture (sulfuric acid and nitric acid)
Raw coal, for the oxidized coal for using nitration mixture to handle as carbon source, polyvinyl alcohol obtains colloidal sol as crosslinking agent and pore creating material, progress aging,
The processes such as freeze-drying obtain xerogel, then the coal base grading-hole charcoal-aero gel with tridimensional network is obtained through high temperature cabonization.
A kind of preparation method of coal base grading-hole charcoal-aero gel of the invention, process are as follows:
(1) it weighs oxidized coal to be added in distilled water, potassium hydroxide is added and is adjusted to solution as neutrality, polyvinyl alcohol is added, 80oC
Under continuously stir 12 hours, obtain colloidal sol.Colloidal sol is placed on -70 againoIt is freezed 24 hours in the refrigerator of C, then vacuum refrigeration
Dry, finally high temperature cabonization again, obtains coal base grading-hole charcoal-aero gel.
(2) mass ratio of the oxidized coal in step (1) and polyvinyl alcohol is 4:1,4:2,4:4.
(3) amount of the distilled water in step (1) is respectively 8 milliliters, 10 milliliters, 12 milliliters.
(4) carburizing temperature in step (1) is 700oC, 800oC, 900oC, soaking time are 2 hours, heating rate
It is 5oC/min, protection gas are nitrogen.
A kind of preparation method with tridimensional network coal base grading-hole charcoal-aero gel of the invention.
The utility model has the advantages that
(1) Xinjiang coal resources abundant are utilized, cheap, synthesis process is simple, is a kind of chemical preparation process of green.
(2) experimental design is ingenious: macromolecular coal being cut into the oxidized coal of small molecule using nitration mixture, dissolves it in distillation
In water, oxidized coal forms collosol and gel as carbon source, polyvinyl alcohol cross-linking together, is carbonized through a step, polyvinyl alcohol point
It solves pore-creating and is not necessarily to subsequent processing, the coal base grading-hole charcoal-aero gel with tridimensional network is made.
Detailed description of the invention:
What Fig. 1 was obtained has tridimensional network coal base grading-hole charcoal-aero gel (a) macroscopic view (carbonization front and back)；(b, c) SEM figure
(microscopic appearance)
Specific implementation method:
Below with reference to specific example, the present invention is further explained.
Coal, Xinjiang Heishan；The concentrated sulfuric acid, nitric acid are bought in Tianjin Yong Sheng Fine Chemical Co., Ltd；Polyvinyl alcohol, I
Fourth reagent (Shanghai) Co., Ltd.；Potassium hydroxide, Tianjin Fu Chen Fine Chemical Co., Ltd；
Example 1:
(1) the Xinjiang Heishan coal for weighing 10 grams of 200 mesh sieve of mistake is raw material, is placed in 5 liters of large beaker, in ice-water bath (0-5oC under the conditions of), by nitration mixture (sulfuric acid and nitric acid) (volume ratio=V according to a certain percentageSulfuric acid:VNitric acid=3:1, totally 180 milliliters) several times
It rapidly joins, with the mechanical stirring of certain revolving speed until nitration mixture is added completely into, then it is stirred 20-30 minutes in ice-water bath；
Then 250 milliliters of distilled water is added several times, is followed by stirring for 2-3 hours, is eventually adding distilled water to 5 milliliters, stands overnight.
Then it filters, filter cake is collected, 110o12 hours are dried in the convection oven of C to doing, and obtain oxidized coal.
(2) oxidized coal for weighing 0.8 gram is dispersed in 10 milliliters of distilled water, and a certain amount of potassium hydroxide is added and adjusts
Solution adds 0.4 gram of polyvinyl alcohol to neutrality, and 80oC heating stirring 12 hours, colloidal sol is obtained, finally places sample
- 70oIt is freezed 24 hours in the refrigerator of C, using freeze-drying, obtains xerogel.
(3) xerogel in step (2) is placed in Noah's ark, is placed in tube furnace, is carbonized.Carburizing temperature is 800oC, soaking time are 2 hours, finally obtain coal base grading-hole charcoal-aero gel, are denoted as HPCAs4-10-800.
Fig. 1 shows: the microscopic appearance of obtained coal base grading-hole charcoal-aero gel, is the three-dimensional cross-linked network with grading-hole
Shape structure.
Embodiment 2:
The amount of polyvinyl alcohol in embodiment 1 is changed to 0.2 gram, remaining operation finally obtains coal base grading-hole charcoal with embodiment 1
Aeroge is denoted as HPCAs2-10-800.
Embodiment 3:
The amount of polyvinyl alcohol in embodiment 1 is changed to 0.8 gram, remaining operation finally obtains coal base grading-hole charcoal with embodiment 1
Aeroge is denoted as HPCAs8-10-800.
Embodiment 4:
Carburizing temperature in embodiment 1 is changed to 700oC, remaining operation finally obtain coal base grading-hole charcoal gas with embodiment 1
Gel is denoted as HPCAs4-10-700.
Embodiment 5:
Carburizing temperature in embodiment 1 is changed to 900oC, remaining operation finally obtain coal base grading-hole charcoal gas with embodiment 1
Gel is denoted as HPCAs4-10-900.
Embodiment 6:
The amount of distilled water in embodiment 1 is changed to 8 milliliters, remaining operation finally obtains coal base grading-hole charcoal gas with embodiment 1
Gel is denoted as HPCAs4-8-800.
Embodiment 7:
The amount of distilled water in embodiment 1 is changed to 12 milliliters, remaining operation finally obtains coal base grading-hole charcoal with embodiment 1
Aeroge is denoted as HPCAs4-12-800.
Claims (8)
1. one kind has tridimensional network coal base grading-hole charcoal-aero gel, which is characterized in that cut macromolecular coal using nitration mixture
It is cut into the oxidized coal of small molecule, is dissolved it in distilled water, oxidized coal is as carbon source, polyvinyl alcohol cross-linking shape together
It at collosol and gel, is carbonized through a step, polyvinyl alcohol decomposes pore-creating and is not necessarily to subsequent processing, and the coal base with tridimensional network is made
Grading-hole charcoal-aero gel.
2. a kind of preparation method with tridimensional network coal base grading-hole charcoal-aero gel, comprising:
(1) the Xinjiang Heishan coal for weighing 10 grams of 200 mesh sieve of mistake is raw material, is placed in 5 liters of large beaker, in ice-water bath (0-5oC under the conditions of), by nitration mixture (sulfuric acid and nitric acid) (volume ratio=V according to a certain percentageSulfuric acid:VNitric acid=3:1, totally 180 milliliters) several times
It rapidly joins, with the mechanical stirring of certain revolving speed until nitration mixture is added completely into, then it is stirred 20-30 minutes in ice-water bath；
Then 250 milliliters of distilled water is added several times, is followed by stirring for 2-3 hours, is eventually adding distilled water to 5 liters, stands overnight；
Then it filters, filter cake is collected, 110o12 hours are dried in the convection oven of C to doing, and obtain oxidized coal；
(2) 0.8 gram of oxidized coal is weighed obtained in step (1), is dispersed in 10 milliliters of distilled water, a certain amount of hydrogen-oxygen is added
Change potassium and adjust solution to neutrality, adds 0.4 gram of polyvinyl alcohol, 80 oCHeating stirring 12 hours, colloidal sol is obtained, then by sample
Product are placed on -70oIt is freezed in the refrigerator of C 24 hours, finally by freeze-drying, obtains xerogel；
(3) xerogel in step (2) is placed in Noah's ark, is subsequently placed in tube furnace, is carbonized；Carburizing temperature is
800 oC, soaking time are 2 hours, finally obtain coal base grading-hole charcoal-aero gel, are denoted as HPCAs4-10-800.
3. in the method according to claim 2 for preparing coal base grading-hole charcoal-aero gel, it is characterised in that:
Carburizing temperature described in step (3) is respectively 700oC, 800oC, 900oC, carbonization time are 2 hours, the guarantor
Shield gas is nitrogen, heating rate 5oC/min。
4. in the method according to claim 2 for preparing coal base grading-hole charcoal-aero gel, it is characterised in that:
The mass ratio of oxidized coal and polyvinyl alcohol in step (2) is 4:1,4:2,4:4.
5. in the method according to claim 2 for preparing coal base grading-hole charcoal-aero gel, it is characterised in that: in step (2)
The amount of distilled water be respectively 8 milliliters, 10 milliliters, 12 milliliters.
6. in the method according to claim 2 for preparing coal base grading-hole charcoal-aero gel, it is characterised in that:
The mechanical stirring revolving speed of processing coal in step (1) is 300-600 r/min, and 20-30 is stirred after being added completely into acid
Minute；When nitration mixture is added, it should rapidly join (30 milliliters are added every time) several times, guarantee the oxidation quality of coal；It is being added
Continue stirring 2-3 hours after distilled water, aoxidizes coal adequately.
7. a kind of coal base grading-hole charcoal-aero gel with tridimensional network, it is characterised in that by appointing described in power 1-6
One method preparation gained.
8. as claimed in claim 7 is with tridimensional network coal base grading-hole charcoal-aero gel.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115285981A (en) * | 2022-09-01 | 2022-11-04 | 西安交通大学 | Preparation method and application of graphene quantum dot aerogel derived porous carbon |
-
2019
- 2019-03-11 CN CN201910178612.2A patent/CN109956460A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115285981A (en) * | 2022-09-01 | 2022-11-04 | 西安交通大学 | Preparation method and application of graphene quantum dot aerogel derived porous carbon |
| CN115285981B (en) * | 2022-09-01 | 2023-08-15 | 西安交通大学 | Preparation method and application of graphene quantum dot aerogel-derived porous carbon |
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