CN109317063A - A kind of charcoal-aero gel and preparation method thereof - Google Patents

A kind of charcoal-aero gel and preparation method thereof Download PDF

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CN109317063A
CN109317063A CN201811522335.4A CN201811522335A CN109317063A CN 109317063 A CN109317063 A CN 109317063A CN 201811522335 A CN201811522335 A CN 201811522335A CN 109317063 A CN109317063 A CN 109317063A
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resorcinol
formaldehyde
charcoal
conditions
under
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CN109317063B (en
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张海礁
刘鑫博
颜彤宇
吴岩
孙俭峰
周长海
周波
黄耀群
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Heilongjiang University of Science and Technology
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Heilongjiang University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0091Preparation of aerogels, e.g. xerogels
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The present invention discloses a kind of charcoal-aero gel and preparation method thereof, is related to Carbon Materials preparation field, and the preparation method of the charcoal-aero gel includes: that resorcinol and formaldehyde are dissolved in water, reacts under the conditions of basic catalyst, forms resorcinol-formaldehyde solution;By the resorcinol-formaldehyde solution left standstill, resorcinol-formaldehyde gel rubber system is formed;The resorcinol-formaldehyde gel rubber system is freezed under the conditions of -120 DEG C~-170 DEG C, forms resorcinol-formaldehyde jelly system;After the resorcinol-formaldehyde jelly system is dried in vacuo, it is placed in graphite jig;The graphite jig is put into discharge plasma sintering furnace after being sintered under vacuum condition, it is cooling, obtain the charcoal-aero gel.The preparation method of charcoal-aero gel provided by the invention, it is smaller to the microstructural damage of carbon aerogel material mesoporous in preparation process, while the carbon aerogel material prepared has pore structure, and pore structure is in the distribution of continuous gradient state.

Description

A kind of charcoal-aero gel and preparation method thereof
Technical field
The present invention relates to Carbon Materials preparation fields, and in particular to a kind of charcoal-aero gel and preparation method thereof.
Background technique
Charcoal-aero gel is due to low-density, high-specific surface area and continuous pore structure and good high temperature resistant and resistance to Etching characteristic has a wide range of applications in absorption and catalytic field, and potential application value causes the pole of researcher Big interest.Currently, the existing charcoal-aero gel method for preparing focuses primarily upon high temperature cabonization method, using under inert gas protection or very Organic precursor is heated in high temperature furnace under empty condition, is carbonized, carbon aerogel material is made;But above-mentioned preparation method system Standby charcoal-aero gel pore structure is irregular, seriously constrains absorption and the filtering feature of carbon aerogel material.
In view of the above drawbacks, creator of the present invention obtains the present invention by prolonged research and practice finally.
Summary of the invention
To solve above-mentioned technological deficiency, the technical solution adopted by the present invention is, provides a kind of preparation side of charcoal-aero gel Method includes the following steps:
Resorcinol and formaldehyde are dissolved in water, reacted under the conditions of basic catalyst, resorcinol-formaldehyde solution is formed;
By the resorcinol-formaldehyde solution left standstill, resorcinol-formaldehyde gel rubber system is formed;
The resorcinol-formaldehyde gel rubber system is freezed under the conditions of -120 DEG C~-170 DEG C, forms resorcinol-first Aldehyde Gel system;
After the resorcinol-formaldehyde jelly system is dried in vacuo, it is placed in graphite jig;
The graphite jig is put into discharge plasma sintering furnace after being sintered under vacuum condition, it is cooling, it obtains To the charcoal-aero gel.
Optionally, described that resorcinol and formaldehyde are dissolved in water, under the conditions of basic catalyst reaction include:
2-10g resorcinol and 8-16ml formaldehyde are dissolved in 20-100ml distilled water, adjust pH value between 7-11, shape At mixed solution;
0.04-1g sodium carbonate is added into the mixed solution, is stirred to react 1-2h at room temperature.
Optionally, it is described by the resorcinol-formaldehyde solution left standstill include: by the resorcinol-formaldehyde solution in It stands under the conditions of 50 DEG C, is then stood under the conditions of 80 DEG C.
Optionally, time that the resorcinol-formaldehyde solution is stood under the conditions of 50 DEG C and in 80 DEG C of items The time stood under part is 2-4h.
Optionally, it is described by the resorcinol-formaldehyde gel rubber system freezed under the conditions of -120 DEG C~-170 DEG C when Between be 1-2h.
Optionally, it is described by the resorcinol-formaldehyde jelly system carry out vacuum drying include: by the isophthalic two Phenol-formaldehyde jelly system is dried in vacuo under the conditions of -40 DEG C~-120 DEG C, is then dried in vacuo under the conditions of 150 DEG C -200 DEG C.
Optionally, described that the resorcinol-formaldehyde jelly system is vacuum drying under the conditions of -40 DEG C~-120 DEG C Time is 4-6h, and the vacuum drying time is 2-6h under the conditions of 150 DEG C -200 DEG C.
Optionally, the described graphite jig is put into discharge plasma sintering furnace is sintered under vacuum condition It include: that the graphite jig is put into discharge plasma sintering furnace under vacuum condition, with 50~150 DEG C/minute of speed 800~1200 DEG C are warming up to, keeps the temperature 5~10 minutes.
Another object of the present invention is to provide a kind of charcoal-aero gel, the charcoal-aero gel by above-mentioned charcoal-aero gel system Preparation Method is made.
Optionally, the charcoal-aero gel has graded pore structure.
Compared with the prior art the beneficial effects of the present invention are:
1, the preparation method of charcoal-aero gel provided by the invention, preparation process is simple, and low energy consumption, short preparation period, preparation It is smaller to the microstructural damage of carbon aerogel material mesoporous in the process, while the carbon aerogel material prepared has pore structure, And pore structure is complete, rule, and is distributed in continuous gradient state.
2, carbon aerogel material prepared by the present invention has pore structure, and pore structure is complete, rule, and is in continuous gradient shape State distribution.
3, the carbon aerogel material prepared by the present invention with continuous gradient pore structure, when being used to adsorb and filter, energy Enough achieve the effect that successively to filter, it can first filter large particulate matter, refilter finely ground particle substance, finally inhaled by microcellular structure Attached micron particles greatly extend charcoal-aero gel material so as to improve absorption and the filtering feature of carbon aerogel material The use scope of material.
Detailed description of the invention
It, below will be to required in embodiment description in order to illustrate more clearly of the technical solution in various embodiments of the present invention The attached drawing used is briefly described.
Fig. 1 is the SEM figure of carbon aerogel material prepared by the present invention;
Fig. 2 is the schematic diagram that the present invention freezes resorcinol-formaldehyde gel rubber system;
Fig. 3 is the flow chart of carbon aerogel material prepared by the present invention.
Specific embodiment
Below in conjunction with attached drawing, the forgoing and additional technical features and advantages are described in more detail.
Preparation method for the current charcoal-aero gel of solution is larger to the microstructural damage of carbon aerogel material, to restrict The problem of absorption of carbon aerogel material obtained and filtering feature, the present invention provide a kind of preparation method of charcoal-aero gel, lead to It crosses and prepares resorcinol-formaldehyde gel rubber system, resorcinol-formaldehyde gel rubber system is freezed, resorcinol-formaldehyde is made Jelly system, then resorcinol-formaldehyde jelly system is placed in graphite jig in discharge plasma sintering furnace in vacuum Under the conditions of be sintered, it is cooling, obtain charcoal-aero gel.Charcoal-aero gel prepared by the present invention has pore structure, and the pore structure has There is continuous gradient, so that the pore structure of charcoal-aero gel prepared by the present invention is regular, so as to improve carbon aerogel material Absorption and filtering feature.
Shown in Figure 3, the preparation method of charcoal-aero gel provided by the invention specifically includes:
Resorcinol and formaldehyde are dissolved in water, reacted under the conditions of basic catalyst, resorcinol-formaldehyde solution is formed;
By resorcinol-formaldehyde solution left standstill, resorcinol-formaldehyde gel rubber system is formed;
Resorcinol-formaldehyde gel rubber system is freezed under the conditions of -120 DEG C~-170 DEG C, resorcinol-formaldehyde is formed and freezes Colloid system;
After resorcinol-formaldehyde jelly system is dried in vacuo, it is placed in graphite jig;
Graphite jig is put into discharge plasma sintering furnace after being sintered under vacuum condition, it is cooling, obtain charcoal Aeroge.
In above-mentioned preparation method, resorcinol is mixed under the conditions of basic catalyst with formaldehyde first, resorcinol with Polycondensation reaction occurs for formaldehyde, after forming resorcinol-formaldehyde (RF) solution, further by resorcinol-formaldehyde solution obtained It is stood, the chemical bond during standing in adjacent polycondensation product is combined, and polycondensation reaction continues;As polycondensation is anti- The progress answered, the molecular weight of product is increasing, and the viscosity of resorcinol-formaldehyde solution is also gradually increased, until product loses Mobility forms resorcinol-formaldehyde gel rubber system;The by-product wherein generated in the hydrone in solution and reaction process The small-molecule substances such as the impurity in object, raw material are as the carry out uniform settlement of reaction is in resorcinol-formaldehyde gel rubber system.
Resorcinol and formaldehyde are wherein dissolved in water, under the conditions of basic catalyst reaction include:
2g-10g resorcinol and 8ml-16ml formaldehyde are dissolved in 20ml-100ml distilled water, adjust pH value 7-11 it Between, form mixed solution;
0.04g-1g basic catalyst is added into mixed solution, is stirred to react 1-2h at room temperature.
Wherein adjust pH value method use the common pH value adjusting method of chemical field, the present invention preferably by The NaOH solution of 0.1mol/L adjusts pH value.
Neutral and alkali catalyst of the present invention is sodium carbonate or potassium carbonate, and the preferred basic catalyst of the present invention is sodium carbonate.To make Reactant can be uniformly mixed, and sufficiently be reacted, and after mixed solution is added in catalyst, be stirred, to improve turning for reactant Rate.
To make resorcinol-formaldehyde solution obtained be converted into gel rubber system, resorcinol-formaldehyde solution is carried out quiet Certain time is set, to promote polycondensation reaction to carry out, ultimately forms gel rubber system.Due to the reaction of polycondensation reaction at different temperatures The molecular weight of speed and polycondensation product is different, for the defect for reducing the pore structure generated in gel rubber system forming process, keeps away Exempt to damage the microstructure of pore structure, it is in charcoal-aero gel preparation method provided by the invention that resorcinol-formaldehyde is molten Liquid standing includes: to stand resorcinol-formaldehyde solution under the conditions of 50 DEG C, is then stood under the conditions of 80 DEG C, wherein by between Time that benzenediol-formalin is stood under the conditions of 50 DEG C and the time stood under the conditions of 80 DEG C are 2-4h.
Resorcinol-formaldehyde gel rubber system obtained is subjected to cryogenic refrigeration under the conditions of -120 DEG C~-170 DEG C, due to Temperature reduces rapidly, and is combined between adjacent molecule by Van der Waals force in resorcinol-formaldehyde gel rubber system, forms spatial networks knot Structure, hydrone and other impurities small-molecule substance are scattered in the gap of reticular structure, form resorcinol-formaldehyde frozen glue body System.Since in refrigerating process, chilling rate is internally gradually decreased by the surface of resorcinol-formaldehyde jelly system, thus Freezing degree is caused internally to gradually decrease from resorcinol-formaldehyde jelly system surface, so that the space networks formed in system The gap of shape structure is internally gradually reduced by surface, and is distributed in continuous gradient.The present invention preferably coagulates resorcinol-formaldehyde The time that colloid freezes under the conditions of lying in -120 DEG C~-170 DEG C is 1-2h.
The mode for carrying out cryogenic refrigeration, which can be used, is put into resorcinol-formaldehyde gel rubber system in the container for being equipped with cold source, The container low temperature environment is placed in again to get off to freeze, it is shown in Figure 2.
Further the resorcinol-formaldehyde jelly system of preparation is dried in vacuo, hydrone is removed and impurity is small After molecule, resorcinol-formaldehyde jelly system is placed in graphite jig, in vacuum condition in discharge plasma sintering furnace Under be sintered;The characteristic that graphite is utilized in sintering process, by way of plasma heating, from resorcinol-first Heating inside Aldehyde Gel system, moment generate high temperature, provocative reaction activity, so that resorcinol-formaldehyde jelly system moment charcoal Change forms spacial framework, while by-product volatilizees at high temperature;After cooling, carbon aerogel material is obtained.
Since the gap of the space net structure formed in resorcinol-formaldehyde jelly system is internally gradually subtracted by surface It is small, and be distributed in continuous gradient, when being sintered, the gap in resorcinol-formaldehyde jelly system forms cavernous structure, shape At cavernous structure maintain jelly system void be in continuous gradient distribution design feature so that preparation charcoal-aero gel Material has the pore structure of continuous gradient distribution.
Specifically, resorcinol-formaldehyde gel rubber system is freezed 1-2h under the conditions of -120 DEG C~-170 DEG C, isophthalic is made After diphenol-formaldehyde jelly system, it includes: to freeze resorcinol-formaldehyde that resorcinol-formaldehyde jelly system, which is carried out vacuum drying, Colloid is dried in vacuo under the conditions of lying in -40 DEG C~-120 DEG C, is then dried in vacuo under the conditions of 150 DEG C -200 DEG C;The present invention is excellent Choosing by resorcinol-formaldehyde jelly system under the conditions of -40 DEG C~-120 DEG C the vacuum drying time be 4-6h, in 150 DEG C - The vacuum drying time is 2-6h under the conditions of 200 DEG C.
Due to existing simultaneously hydrone and other small molecular weight impurities in resorcinol-formaldehyde gel rubber system, by isophthalic two Phenol-formaldehyde jelly system carries out process of vacuum drying and is divided into the progress of two steps, and vacuum is dry under the conditions of -40 DEG C~-120 DEG C first It is dry, so that the hydrone in jelly system directly distils, remove hydrone;Then it is dried in vacuo under the conditions of 150 DEG C -200 DEG C, Other impurities small molecule than water in jelly system is removed, to reduce the impurity content in carbon aerogel material, improves charcoal The performance of aerogel material, while after impurity in jelly system gap is removed, pore structure is formed, to be further sintered The carbon aerogel material formed afterwards has the pore structure of continuous gradient distribution.
Graphite jig is put into discharge plasma sintering furnace to be sintered under vacuum condition include: by graphite jig It is put into discharge plasma sintering furnace, under vacuum condition, is warming up to 800 DEG C~1200 with 50~150 DEG C/minute of speed DEG C, keep the temperature 5~10 minutes.
It is heated up by the way of ladder-elevating temperature in sintering process, to control heating rate, so that resorcinol-formaldehyde Each ingredient can sufficiently be reacted in jelly system, reduce the generation of side reaction.
The preparation method of charcoal-aero gel provided by the invention has the advantages that low energy consumption, with short production cycle, while preparing Carbon aerogel material pore structure is complete, rule, and is distributed in continuous gradient, so as to improve the absorption of carbon aerogel material with Filtering feature.
Carbon aerogel material with continuous gradient pore structure, for layer-by-layer filtering can be reached when adsorbing and filtering Effect, it can first filter large particulate matter, refilter finely ground particle substance, micron particles are finally adsorbed by microcellular structure, Greatly extend the use scope of carbon aerogel material.
Embodiment one
The present embodiment provides a kind of preparation methods of charcoal-aero gel, specifically comprise the following steps:
S1: 2g resorcinol and 8ml formaldehyde are dissolved in 20ml distilled water, are adjusted pH value to 7, are obtained mixed solution;
S2: 0.04g sodium carbonate is added into mixed solution, is stirred to react 1h at room temperature, obtains resorcinol-formaldehyde Solution;
S3: standing 2h for resorcinol-formaldehyde solution under the conditions of 50 DEG C, and 2h is then stood under the conditions of 80 DEG C, is formed Resorcinol-formaldehyde gel rubber system;
S4: resorcinol-formaldehyde gel rubber system is freezed into 1h under the conditions of -120 DEG C, forms resorcinol-formaldehyde frozen glue System;
S5: being dried in vacuo 4h for resorcinol-formaldehyde jelly system under the conditions of -40 DEG C, then true under the conditions of 150 DEG C The dry 2h of sky, the resorcinol-formaldehyde jelly system after being dried;
S6: the resorcinol-formaldehyde jelly system after drying is placed in graphite jig, and graphite jig is put into electric discharge etc. In gas ions sintering furnace, under vacuum condition, 800 DEG C are warming up to 50 DEG C/minute of speed, heat preservation is after five minutes, cooling, obtains Charcoal-aero gel.
The preparation method of charcoal-aero gel provided in this embodiment, through resorcinol and formaldehyde in the presence of basic catalyst Resorcinol-formaldehyde gel rubber system is generated, after cryogenic refrigeration, forms resorcinol-formaldehyde jelly system;By resorcinol- It after formaldehyde jelly system is further dried in vacuo, is sintered by discharge plasma sintering furnace, carbon aerogel material is made.
Fig. 1 is the electron scanning micrograph (SEM figure) of carbon aerogel material manufactured in the present embodiment, dark color in Fig. 1 Part is pore structure, and light-colored part is charcoal-aero gel skeleton, it can be seen from the figure that dark strip pore structure from top to bottom by Gradual change is thin, it was demonstrated that carbon aerogel material central hole structure manufactured in the present embodiment gradually becomes smaller in aperture from top to bottom, and pore structure is in company Continuous gradient conditions distribution.
The preparation method preparation process of charcoal-aero gel provided in this embodiment is simple, and low energy consumption, prepared by short preparation period It is smaller to the microstructural damage of carbon aerogel material mesoporous in journey, while the carbon aerogel material prepared has pore structure, and Pore structure is complete, regular, and is distributed in continuous gradient state.
Carbon aerogel material with continuous gradient pore structure, for layer-by-layer filtering can be reached when adsorbing and filtering Effect, it can first filter large particulate matter, refilter finely ground particle substance, micron particles are finally adsorbed by microcellular structure, So as to improve absorption and the filtering feature of carbon aerogel material, the use scope of carbon aerogel material is greatly extended.
Embodiment two
What is different from the first embodiment is that the preparation method of charcoal-aero gel includes the following steps: in the present embodiment
S1: 6g resorcinol and 12ml formaldehyde are dissolved in 60ml distilled water, are adjusted pH value to 9, are obtained mixed solution;
S2: 0.7g sodium carbonate being added into mixed solution, is stirred to react 1.5h at room temperature, obtains resorcinol-first Aldehyde solution;
S3: standing 3h for resorcinol-formaldehyde solution under the conditions of 50 DEG C, and 3h is then stood under the conditions of 80 DEG C, is formed Resorcinol-formaldehyde gel rubber system;
S4: freezing 1.5h for resorcinol-formaldehyde gel rubber system under the conditions of -150 DEG C, forms resorcinol-formaldehyde and freezes Colloid system;
S5: being dried in vacuo 5h for resorcinol-formaldehyde jelly system under the conditions of -80 DEG C, then true under the conditions of 180 DEG C The dry 4h of sky, the resorcinol-formaldehyde jelly system after being dried;
S6: the resorcinol-formaldehyde jelly system after drying is placed in graphite jig, and graphite jig is put into electric discharge etc. It is cooling after being warming up to 1000 DEG C, heat preservation 8 minutes with 100 DEG C/minute of speed under vacuum condition in gas ions sintering furnace, it obtains To charcoal-aero gel.
The preparation method preparation process of charcoal-aero gel provided in this embodiment is simple, and low energy consumption, prepared by short preparation period It is smaller to the microstructural damage of carbon aerogel material mesoporous in journey, while the carbon aerogel material prepared has pore structure, and Pore structure is complete, regular, and is distributed in continuous gradient state.
The SEM figure of carbon aerogel material manufactured in the present embodiment is shown in Figure 1, makes a concrete analysis of process referring to embodiment one Part related content, repeats no more herein.
Embodiment three
What is different from the first embodiment is that the preparation method of charcoal-aero gel includes the following steps: in the present embodiment
S1: 10g resorcinol and 16ml formaldehyde are dissolved in 100ml distilled water, are adjusted pH value to 11, are obtained mixing molten Liquid;
S2: 1g sodium carbonate is added into mixed solution, is stirred to react 2h at room temperature, it is molten to obtain resorcinol-formaldehyde Liquid;
S3: standing 4h for resorcinol-formaldehyde solution under the conditions of 50 DEG C, and 4h is then stood under the conditions of 80 DEG C, is formed Resorcinol-formaldehyde gel rubber system;
S4: resorcinol-formaldehyde gel rubber system is freezed into 2h under the conditions of -170 DEG C, forms resorcinol-formaldehyde frozen glue System;
S5: resorcinol-formaldehyde jelly system is dried in vacuo 6h under the conditions of -120 DEG C, then under the conditions of 200 DEG C It is dried in vacuo 6h, the resorcinol-formaldehyde jelly system after being dried;
S6: the resorcinol-formaldehyde jelly system after drying is placed in graphite jig, and graphite jig is put into electric discharge etc. In gas ions sintering furnace, under vacuum condition, 1200 DEG C are warming up to 150 DEG C/minute of speed, heat preservation is after ten minutes, cooling, obtains To charcoal-aero gel.
The preparation method preparation process of charcoal-aero gel provided in this embodiment is simple, and low energy consumption, prepared by short preparation period It is smaller to the microstructural damage of carbon aerogel material mesoporous in journey, while the carbon aerogel material prepared has pore structure, and Pore structure is complete, regular, and is distributed in continuous gradient state.
The SEM figure of carbon aerogel material manufactured in the present embodiment is shown in Figure 1, makes a concrete analysis of process referring to embodiment one Part related content, repeats no more herein.
The foregoing is merely presently preferred embodiments of the present invention, is merely illustrative for the purpose of the present invention, and not restrictive 's.Those skilled in the art understand that in the spirit and scope defined by the claims in the present invention many changes can be carried out to it, It modifies or even equivalent, but falls in protection scope of the present invention.

Claims (10)

1. a kind of preparation method of charcoal-aero gel, which comprises the steps of:
Resorcinol and formaldehyde are dissolved in water, reacted under the conditions of basic catalyst, resorcinol-formaldehyde solution is formed;
By the resorcinol-formaldehyde solution left standstill, resorcinol-formaldehyde gel rubber system is formed;
The resorcinol-formaldehyde gel rubber system is freezed under the conditions of -120 DEG C~-170 DEG C, resorcinol-formaldehyde is formed and freezes Colloid system;
After the resorcinol-formaldehyde jelly system is dried in vacuo, it is placed in graphite jig;
The graphite jig is put into discharge plasma sintering furnace after being sintered under vacuum condition, it is cooling, obtain institute State charcoal-aero gel.
2. the preparation method of charcoal-aero gel as described in claim 1, which is characterized in that described to be dissolved in resorcinol and formaldehyde Water, under the conditions of basic catalyst reaction include:
2-10g resorcinol and 8-16ml formaldehyde are dissolved in 20-100ml distilled water, adjust pH value between 7-11, is formed mixed Close solution;
0.04-1g sodium carbonate is added into the mixed solution, is stirred to react 1-2h at room temperature.
3. the preparation method of charcoal-aero gel as described in claim 1, which is characterized in that described by the resorcinol-formaldehyde Solution left standstill includes: to stand the resorcinol-formaldehyde solution under the conditions of 50 DEG C, is then stood under the conditions of 80 DEG C.
4. the preparation method of charcoal-aero gel as claimed in claim 3, which is characterized in that described by the resorcinol-formaldehyde Time that solution is stood under the conditions of 50 DEG C and the time stood under the conditions of 80 DEG C are 2-4h.
5. the preparation method of charcoal-aero gel as described in claim 1, which is characterized in that described by the resorcinol-formaldehyde The time that gel rubber system freezes under the conditions of -120 DEG C~-170 DEG C is 1-2h.
6. the preparation method of charcoal-aero gel as described in claim 1, which is characterized in that described by the resorcinol-formaldehyde Jelly system carry out vacuum drying include: by the resorcinol-formaldehyde jelly system under the conditions of -40 DEG C~-120 DEG C vacuum It is dry, then it is dried in vacuo under the conditions of 150 DEG C -200 DEG C.
7. the preparation method of charcoal-aero gel as claimed in claim 6, which is characterized in that described by the resorcinol-formaldehyde Jelly system vacuum drying time under the conditions of -40 DEG C~-120 DEG C is 4-6h, is dried in vacuo under the conditions of 150 DEG C -200 DEG C Time be 2-6h.
8. the preparation method of charcoal-aero gel as described in claim 1, which is characterized in that described to be put into the graphite jig Be sintered under vacuum condition in electro-plasma sintering furnace includes: that the graphite jig is put into discharge plasma sintering In furnace under vacuum condition, 800~1200 DEG C are warming up to 50~150 DEG C/minute of speed, keeps the temperature 5~10 minutes.
9. a kind of charcoal-aero gel, which is characterized in that the charcoal-aero gel is by the described in any item charcoal-aero gels of claim 1-8 Preparation method is made.
10. charcoal-aero gel as claimed in claim 9, which is characterized in that the charcoal-aero gel has graded pore structure.
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