CN108862239A - A kind of preparation method of high tenacity charcoal-aero gel - Google Patents
A kind of preparation method of high tenacity charcoal-aero gel Download PDFInfo
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- CN108862239A CN108862239A CN201811135114.1A CN201811135114A CN108862239A CN 108862239 A CN108862239 A CN 108862239A CN 201811135114 A CN201811135114 A CN 201811135114A CN 108862239 A CN108862239 A CN 108862239A
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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 technical field of preparation for inorganic material, and in particular to a kind of preparation method of high tenacity charcoal-aero gel.Ramee is made by raw material of ramie first in the present invention, ramee after hydro-thermal process is obtained into modified ramie Carbon fibe with sodium silicate solution blending reaction, as high tenacity charcoal-aero gel, the present invention obtains ramee by raw material of ramie first, again by ramee base extraction, so that the elastic recovery of ramee enhances, toughness is promoted, curling and hook epistasis improve, cohesive force enhancing, improve the wearability of ramee, using isopropanol as alkylating agent, greatly strengthen bulking capacity, improve presently, there are the defect that can shrink of carbon aerogel material, orthosilicic acid solution obtained is heated into reaction and generates nano silica, nano silica can improve the anti-aging of charcoal-aero gel, intensity and chemical-resistance, used raw material does not have toxicity, meet environmental requirement, it has broad application prospects.
Description
Technical field
The present invention relates to technical field of preparation for inorganic material, and in particular to a kind of preparation method of high tenacity charcoal-aero gel.
Background technique
Aeroge is the porosity amorphous solid material being made of nanoscale colloidal particle or the high-polymer molecule, and at present
Most light condensed state material in synthetic material.Its unique nanometer porous structure of opening and continuous three-dimensional network, are allowed to
With extremely low density, high-specific surface area and high porosity, show strong adsoption catalysis ability, lower thermal conductivity, low acoustic impedance and
The characteristics such as low-refraction, therefore aeroge has become good catalyst and its carrier, adsorbent and gas filtering material.
Traditional aerogel material silica, aluminium oxide, silica-alumina, resorcinol-formaldehyde（RF）With charcoal gas
Gel etc., wherein charcoal-aero gel is a kind of light nanoporous material with crosslinking shape structure, voidage height, specific surface area
Greatly, variable density range is wide, structure is adjustable, in fields such as high temperature insulating, electrode material, catalyst, wastewater treatment and target materials
It has broad application prospects, it has also become the research hot topic of aeroge field in recent years.
Existing charcoal-aero gel preparation method is generally with resorcinol-formaldehyde system, phenol-formaldehyde system or phenol-chaff
Aldehyde system is base stock, and polycondensation reaction then occurs under the base catalysis of sodium carbonate, magnesium acetate or hexamethylenetetramine, is passed through
RF aeroge is made after gel aging, exchange of solvent and supercritical drying processing, finally carries out high temperature carbonization under an inert atmosphere
Processing obtains the charcoal-aero gel for being able to maintain its tridimensional network.The whole preparation process period is long, at high cost, is unfavorable for industry
Production, and the part collapsing during supercritical drying and Pintsch process due to charcoal-aero gel skeleton will lead to material and receive
Contracting, and cause the size of material not easy to control.Since charcoal-aero gel is in single bulk more, there is also elasticity is very poor and should not process
The defects of.In addition, the raw material for preparing charcoal-aero gel at present is almost the strong chemicals of toxicity, such as phenol, six methines four
Amine and acetonitrile etc. are easy to cause larger pollution to environment, limit the development and application of charcoal-aero gel to a certain extent.
The charcoal-aero gel of existing method preparation the problems such as that there are intensity is low, and brittleness is big, and porous structure is difficult to control, moreover,
The preparation method period of conventional method charcoal-aero gel is long, and at high cost, toxicity is big.Therefore, develop low cost, short manufacturing cycle,
The charcoal-aero gel of high homogenieity is of great significance.
Summary of the invention
Present invention mainly solves the technical issues of, for presently, there are carbon aerogel material be easy to happen contraction, elasticity
Poor, used raw material will cause the defect of larger pollution to environment, provide a kind of preparation method of high tenacity charcoal-aero gel.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that：
A kind of preparation method of high tenacity charcoal-aero gel, it is characterised in that specifically preparation step is：
（1）Take ramie leaf to be put into steam-explosion jar, and be passed through steam into steam-explosion jar, until in steam-explosion jar pressure up to 2.5~
After 2.8MPa, 40~50s of pressure maintaining, steam-explosion jar discharge valve is opened, is injected into material moment in steam-explosion jar in receiving tank, received
Collect material in receiving tank, obtains ramee；
（2）Above-mentioned ramee, sodium hydroxide solution and aqueous isopropanol are put into blender, with 600~800r/min
Revolving speed stir 15~20min, obtain modified ramie；
（3）Modified ramie is put into autoclave, temperature and pressure in setting autoclave, hydro-thermal 2~3h of carbonization reaction,
It discharges after reaction, obtains modified ramie Carbon fibe；
（4）Above-mentioned modified ramie Carbon fibe is put into beaker bottom, sodium silicate solution is added into beaker, then be added into beaker
Hydrochloric acid, adjusting pH is 4~5, obtains mixed liquor；
（5）Mixed liquor obtained above is poured into reaction kettle, 1~2h is stirred to react, after reaction, discharging is put into baking oven
In, it discharges at 105~110 DEG C after dry 1~2h to get high tenacity charcoal-aero gel.
Step（1）The temperature of the steam is 200~250 DEG C.
Step（2）The mass ratio of the above-mentioned ramee, sodium hydroxide solution and aqueous isopropanol is 10 ︰, 10 ︰
1, the score of sodium hydroxide solution quality is 40%, and the mass fraction of aqueous isopropanol is 50%.
Step（3）Temperature is 200~300 DEG C in the autoclave, and pressure is 0.1~0.2MPa.
Step（4）The quality of the sodium silicate solution is equal with ramie Carbon fibe quality, the quality point of sodium silicate solution
Number is 50%, and the mass fraction of hydrochloric acid is 40%.
Step（5）The temperature of the reaction kettle is 80~90 DEG C.
The beneficial effects of the invention are as follows：
Ramee is made by raw material of ramie first in the present invention, is modified using lye and alkylating agent to it, makes its fiber
The spacing of plain macromolecular increases, and avoids the recrystallization of cellulosic molecule, then carries out hydro-thermal charing to modified ramie,
Porous structure is made it have, the ramee and sodium silicate solution blending reaction after hydro-thermal process obtain being combined with nanometer two
The modified ramie Carbon fibe of silica, as high tenacity charcoal-aero gel, the present invention obtain ramee by raw material of ramie first,
Ramee is tough and tensile, intensity is big, antibacterial bacteriostatic, then by ramee base extraction, after base extraction, base molecule and cellulose
The hydroxy combining of macromolecular reduces cellulose hydrogen bond and weakens with molecular separating force, and the spacing of cellulose macromolecule increases, so that ramie
The elastic recovery enhancing of flaxen fiber, toughness promote, crimp and hook epistasis raising, cohesive force enhancing, improve ramee
Wearability so that ramee is generated alkylated reaction using isopropanol as alkylating agent, ramee is alkylated in concentrated base,
Bulking capacity is greatly strengthened, due to the presence of alkyl, ramee molecule is prevented close to hydrogen bond is formed, to avoid fibre again
The recrystallization for tieing up plain molecule, improve presently, there are the defect that can shrink of carbon aerogel material, by modified ramie
Hydro-thermal charing process is carried out, so that ramee forms porous structure, so that charcoal-aero gel has porous structure and toughness mentions
It rises, sodium metasilicate reacts in acid condition can be made orthosilicic acid precipitating, and orthosilicic acid solution obtained is heated reaction generation and is received
Rice silica, so that nano silica is integrated to ramee surface, nano silica can improve the anti-of charcoal-aero gel
Aging, intensity and chemical-resistance have reticular structure, and porosity is high, and large specific surface area, solar heat protection heat insulation is excellent, this hair
Raw material used in bright does not have toxicity, and there are no pollution to the environment, meets environmental requirement, has broad application prospects.
Specific embodiment
It takes ramie leaf to be put into steam-explosion jar, and is passed through into steam-explosion jar and is preheated to 200~250 DEG C of steam, until steam explosion
Pressure is up to 2.5~2.8MPa in tank, after 40~50s of pressure maintaining, opens steam-explosion jar discharge valve, sprays material moment in steam-explosion jar
Into in receiving tank, material in receiving tank is collected, ramee is obtained；By above-mentioned ramee, the hydrogen-oxygen that mass fraction is 40%
Change the aqueous isopropanol that sodium solution and mass fraction are 50% is that 10 ︰, 10 ︰ 1 is put into blender in mass ratio, with 600~
The revolving speed of 800r/min stirs 15~20min, obtains modified ramie；Modified ramie is put into autoclave, is arranged
Temperature is 200~300 DEG C in autoclave, and pressure is 0.1~0.2MPa, and hydro-thermal 2~3h of carbonization reaction discharges after reaction,
Obtain modified ramie Carbon fibe；Above-mentioned modified ramie Carbon fibe is put into beaker bottom, is added and ramie Carbon fibe into beaker
The sodium silicate solution that the equal mass fraction of quality is 50%, then the hydrochloric acid that mass fraction is 40% is added into beaker, adjust pH
It is 4~5, obtains mixed liquor；Mixed liquor obtained above is poured into reaction kettle, under conditions of temperature is 80~90 DEG C, is stirred
1~2h of reaction is mixed, after reaction, discharging is put into baking oven, is discharged at 105~110 DEG C after dry 1~2h to get high-ductility
Property charcoal-aero gel.
Example 1
It takes ramie leaf to be put into steam-explosion jar, and is passed through into steam-explosion jar and is preheated to 200 DEG C of steam, until pressure reaches in steam-explosion jar
After 2.5MPa, pressure maintaining 40s, steam-explosion jar discharge valve is opened, is injected into material moment in steam-explosion jar in receiving tank, collection connects
Material in closed cans, obtains ramee；By above-mentioned ramee, the sodium hydroxide solution that mass fraction is 40% and quality point
Number is that 10 ︰, 10 ︰ 1 is put into blender for 50% aqueous isopropanol in mass ratio, stirs 15min with the revolving speed of 600r/min, obtains
To modified ramie；Modified ramie is put into autoclave, it is 200 DEG C that temperature in autoclave, which is arranged, and pressure is
0.1MPa, hydro-thermal carbonization reaction 2h, discharges after reaction, obtains modified ramie Carbon fibe；By above-mentioned modified ramie Carbon fibe
It is put into beaker bottom, the mass fraction equal with ramie Carbon fibe quality is added into beaker as 50% sodium silicate solution, then to
The hydrochloric acid that mass fraction is 40% is added in beaker, adjusting pH is 4, obtains mixed liquor；Mixed liquor obtained above is poured into reaction
In kettle, under conditions of temperature is 80 DEG C, it is stirred to react 1h, after reaction, discharging is put into baking oven, dry at 105 DEG C
Discharging is after 1h to get high tenacity charcoal-aero gel.
Example 2
It takes ramie leaf to be put into steam-explosion jar, and is passed through into steam-explosion jar and is preheated to 230 DEG C of steam, until pressure reaches in steam-explosion jar
After 2.7MPa, pressure maintaining 45s, steam-explosion jar discharge valve is opened, is injected into material moment in steam-explosion jar in receiving tank, collection connects
Material in closed cans, obtains ramee；By above-mentioned ramee, the sodium hydroxide solution that mass fraction is 40% and quality point
Number is that 10 ︰, 10 ︰ 1 is put into blender for 50% aqueous isopropanol in mass ratio, stirs 17min with the revolving speed of 700r/min, obtains
To modified ramie；Modified ramie is put into autoclave, it is 250 DEG C that temperature in autoclave, which is arranged, and pressure is
0.1MPa, hydro-thermal carbonization reaction 2h, discharges after reaction, obtains modified ramie Carbon fibe；By above-mentioned modified ramie Carbon fibe
It is put into beaker bottom, the mass fraction equal with ramie Carbon fibe quality is added into beaker as 50% sodium silicate solution, then to
The hydrochloric acid that mass fraction is 40% is added in beaker, adjusting pH is 4, obtains mixed liquor；Mixed liquor obtained above is poured into reaction
In kettle, under conditions of temperature is 85 DEG C, it is stirred to react 1h, after reaction, discharging is put into baking oven, dry at 107 DEG C
Discharging is after 1h to get high tenacity charcoal-aero gel.
Example 3
It takes ramie leaf to be put into steam-explosion jar, and is passed through into steam-explosion jar and is preheated to 250 DEG C of steam, until pressure reaches in steam-explosion jar
After 2.8MPa, pressure maintaining 50s, steam-explosion jar discharge valve is opened, is injected into material moment in steam-explosion jar in receiving tank, collection connects
Material in closed cans, obtains ramee；By above-mentioned ramee, the sodium hydroxide solution that mass fraction is 40% and quality point
Number is that 10 ︰, 10 ︰ 1 is put into blender for 50% aqueous isopropanol in mass ratio, stirs 20min with the revolving speed of 800r/min, obtains
To modified ramie；Modified ramie is put into autoclave, it is 300 DEG C that temperature in autoclave, which is arranged, and pressure is
0.2MPa, hydro-thermal carbonization reaction 3h, discharges after reaction, obtains modified ramie Carbon fibe；By above-mentioned modified ramie Carbon fibe
It is put into beaker bottom, the mass fraction equal with ramie Carbon fibe quality is added into beaker as 50% sodium silicate solution, then to
The hydrochloric acid that mass fraction is 40% is added in beaker, adjusting pH is 5, obtains mixed liquor；Mixed liquor obtained above is poured into reaction
In kettle, under the conditions of at a temperature of 90 °C, it is stirred to react 2h, after reaction, discharging is put into baking oven, dry at 110 DEG C
Discharging is after 2h to get high tenacity charcoal-aero gel.
The charcoal-aero gel that comparative example is produced with Shanghai City company is as a comparison case to high tenacity charcoal produced by the present invention
Charcoal-aero gel in aeroge and comparative example is detected, and testing result is as shown in table 1：
Surface area, opening size test
It is tested using adsorption instrument.
Young's modulus test
It is detected using static method.Static method refers to the one constant bending stress of application on sample, measures its elastic bending
Amount of deflection, or apply a constant stretching on sample（Or compression）Stress measures its elastic deformation amount, or according to stress and answers
Become and calculates elasticity modulus.
1 performance measurement result of table
According to data in table 1 it is found that high tenacity charcoal-aero gel produced by the present invention, has good integrality, density is lower,
Intensity is high, and elasticity is good, good mechanical performance, and raw materials are natural material, and phenol, hexamethylenetetramine and second is not used
The toxic chemicals such as nitrile, therefore any harmful toxic matter will not be generated, there is wide prospect of the application.
Claims (6)
1. a kind of preparation method of high tenacity charcoal-aero gel, it is characterised in that specifically preparation step is：
（1）Take ramie leaf to be put into steam-explosion jar, and be passed through steam into steam-explosion jar, until in steam-explosion jar pressure up to 2.5~
After 2.8MPa, 40~50s of pressure maintaining, steam-explosion jar discharge valve is opened, is injected into material moment in steam-explosion jar in receiving tank, received
Collect material in receiving tank, obtains ramee；
（2）Above-mentioned ramee, sodium hydroxide solution and aqueous isopropanol are put into blender, with 600~800r/min
Revolving speed stir 15~20min, obtain modified ramie；
（3）Modified ramie is put into autoclave, temperature and pressure in setting autoclave, hydro-thermal 2~3h of carbonization reaction,
It discharges after reaction, obtains modified ramie Carbon fibe；
（4）Above-mentioned modified ramie Carbon fibe is put into beaker bottom, sodium silicate solution is added into beaker, then be added into beaker
Hydrochloric acid, adjusting pH is 4~5, obtains mixed liquor；
（5）Mixed liquor obtained above is poured into reaction kettle, 1~2h is stirred to react, after reaction, discharging is put into baking oven
In, it discharges at 105~110 DEG C after dry 1~2h to get high tenacity charcoal-aero gel.
2. a kind of preparation method of high tenacity charcoal-aero gel according to claim 1, it is characterised in that：Step（1）It is described
Steam temperature be 200~250 DEG C.
3. a kind of preparation method of high tenacity charcoal-aero gel according to claim 1, it is characterised in that：Step（2）It is described
Above-mentioned ramee, sodium hydroxide solution and aqueous isopropanol mass ratio be 10 ︰, 10 ︰ 1, sodium hydroxide solution quality
Score is 40%, and the mass fraction of aqueous isopropanol is 50%.
4. a kind of preparation method of high tenacity charcoal-aero gel according to claim 1, it is characterised in that：Step（3）It is described
Autoclave in temperature be 200~300 DEG C, pressure be 0.1~0.2MPa.
5. a kind of preparation method of high tenacity charcoal-aero gel according to claim 1, it is characterised in that：Step（4）It is described
Sodium silicate solution quality it is equal with ramie Carbon fibe quality, the mass fraction of sodium silicate solution is 50%, the quality point of hydrochloric acid
Number is 40%.
6. a kind of preparation method of high tenacity charcoal-aero gel according to claim 1, it is characterised in that：Step（5）It is described
Reaction kettle temperature be 80~90 DEG C.
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Cited By (2)
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| CN113773043A (en) * | 2021-07-14 | 2021-12-10 | 中国科学院金属研究所 | Preparation method of low-density carbon fiber reinforced carbon aerogel composite material |
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Application publication date: 20181123 |