CN108298519A - A kind of preparation method using the enhanced charcoal-aero gel of Ludox - Google Patents
A kind of preparation method using the enhanced charcoal-aero gel of Ludox Download PDFInfo
- Publication number
- CN108298519A CN108298519A CN201810289595.5A CN201810289595A CN108298519A CN 108298519 A CN108298519 A CN 108298519A CN 201810289595 A CN201810289595 A CN 201810289595A CN 108298519 A CN108298519 A CN 108298519A
- Authority
- CN
- China
- Prior art keywords
- charcoal
- ludox
- enhanced
- gel
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
Abstract
The present invention relates to technical field of preparation for inorganic material, and in particular to a kind of preparation method using the enhanced charcoal-aero gel of Ludox.The present invention makes by oneself to obtain thick wood fiber powder using poplar as raw material,Thick wood fiber powder is obtained into wooden nano-cellulose by processing,By Ludox,Salpeter solution and absolute ethyl alcohol are mixed to get mixed liquor,Then to normal heptane,Mixed liquor is added dropwise in the mixture of n-butanol and sucrose ester,Ammonium hydroxide,Reaction is separated by filtration to obtain filter cake,Gel micro-ball finally will be obtained after Washing of Filter Cake,Gel micro-ball is obtained into the enhanced charcoal-aero gel of Ludox by processing,Utilize the affine performance of Ludox and fiber,Reinforcing fiber pore structure,To make the intensity of charcoal-aero gel improve,When wooden nano-cellulose is dispersed in water,Three-dimensional net structure can be formed by interfibrous hydrogen bond and long stapled entanglement,Obtain stable hydrogel,Fiber provides the network skeleton of aeroge stabilization,Improve the intensity and film amount of aeroge,It has a extensive future.
Description
Technical field
The present invention relates to technical field of preparation for inorganic material, and in particular to a kind of using the enhanced charcoal-aero gel of Ludox
Preparation method.
Background technology
Aeroge is the porosity amorphous solid material being made of nanoscale colloidal particle or high-polymer molecular, 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 are 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 aeroges are made after gel aging, exchange of solvent and supercritical drying processing, finally carry out high temperature carbonization under an inert atmosphere
Processing obtains to keep the charcoal-aero gel of its tridimensional network.The whole preparation process period is long, of high cost, is unfavorable for industry
Production, and material can be caused to receive since the part of charcoal-aero gel skeleton caves in during supercritical drying and Pintsch process
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 problems such as that there are intensity is low for charcoal-aero gel prepared by existing method, 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 of high cost, toxicity is big.Therefore, develop low cost, short manufacturing cycle,
The charcoal-aero gel of high homogenieity is of great significance.
Invention content
Present invention mainly solves the technical issues of, that there are intensity is low for the charcoal-aero gel prepared for current existing method, crisp
The problems such as property is big, and porous structure is difficult to control, moreover, the raw material toxicity that conventional method prepares charcoal-aero gel is big
Defect, provide a kind of preparation method using the enhanced charcoal-aero gel of Ludox.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method using the enhanced charcoal-aero gel of Ludox, it is characterised in that specifically preparation process is：
（1）It takes 200~300g poplars to be put into pulverizer, crushes, cross standard screen, obtain wooden powder, weigh 100~150g wood
Matter powder is placed in Soxhlet extractor, and benzyl carbinol and water are mixed to get benzyl carbinol solution at normal temperatures, then by 300~400mL
Benzyl carbinol solution pours into Soxhlet extractor, and extracting obtains thick wood fiber powder after removing extract；
（2）Thick wood fiber powder is put into beaker, 50~60mL sodium chlorite solutions are added into beaker, with glacial acetic acid solution tune
The pH of solution is saved, isothermal holding repeats aforesaid operations 3~5 times, removes lignin, obtains holocellulose；
（3）Holocellulose is impregnated under the conditions of 90~100 DEG C with 120~150mL sodium hydroxide solutions, heat-insulation soaking filters off
Except filtrate obtains purifying cellulose, purifying cellulose is made into water slurry, is placed in ultrasonic wave plant cell pulverizer ultrasonic
Wooden nano-cellulose is made in processing；
（4）It counts in parts by weight, by 10~15 parts of Ludox, 4~6 parts of salpeter solutions and 16~20 parts of absolute ethyl alcohol mixing add
Enter in beaker, stir, obtain mixed liquor, 100~110 portions of normal heptanes, 4~6 parts of n-butanols and 0.1 are added then to three-necked flask
~0.3 part of sucrose ester；
（5）Mixed liquor is added dropwise to constant pressure funnel in three-necked flask, while starting blender stirring, 4~5 parts of ammonia are added dropwise
Water and the wooden nano-cellulose of 30~40 parts of addition, are stirred to react, the substance in filter flask, and removal filtrate obtains filter cake；
（6）Filter cake is washed 3~5 times with acetone, gel micro-ball is obtained, under the conditions of 60~80 DEG C, with ethyl orthosilicate and nothing
Water-ethanol is mixed to get reinforcing agent, and CO is put into after gel micro-ball is impregnated with reinforcing agent2It is dry in supercritical drying drying system, it obtains
Enhanced aeroge is put into retort and carbonizes by enhanced aeroge, obtains the enhanced charcoal-aero gel of Ludox.
Step（1）The grinding time is 1~2h, and be sieved specification is 200 mesh, and benzyl carbinol mixes at normal temperatures with water
Volume ratio is 2 ︰ 1, and extraction temperature is 80~90 DEG C, and the time is 5~10h.
Step（2）The mass fraction of the sodium chlorite solution is 20%, and glacial acetic acid solution mass fraction is 98%, ice vinegar
The pH that acid solution adjusts solution is 4~5, and the isothermal holding time is 5~7h.
Step（3）The mass fraction of the sodium hydroxide solution is 20%, and the heat-insulation soaking time is 2~3h, water slurry
Mass fraction be 10~20%, the power of supersound process is 1200~1500W, and ultrasonic time is 30~45min, control ultrasound
Frequency is 30~35kHz.
Step（4）The mass fraction of the Ludox is 25%, and the mass fraction of salpeter solution is 5%, and mixing time is
15~20min.
Step（5）The constant pressure funnel drop rate is 3~5mL/min, and speed of agitator is 100~120r/
Min, mixing time are 30~45min, and the mass fraction of ammonium hydroxide is 5%, and it is 10~15min to be stirred to react the time.
Step（6）The ethyl orthosilicate is 1 ︰ 3 with absolute ethyl alcohol mixing quality ratio, and gel micro-ball is impregnated with reinforcing agent
Time be 3~5h, supercritical drying temperature is 70~80 DEG C, and drying time is 20~for 24 hours, control in retort as nitrogen or
Argon gas atmosphere, carbonization temperature are 600~1200 DEG C, and carbonization time is 2~8h.
The beneficial effects of the invention are as follows：
（1）The present invention obtains wooden powder after pulverizing and sieving, wooden powder is placed in Soxhlet extractor using poplar as raw material,
Using benzyl carbinol solution as solvent extraction, thick wood fiber powder is obtained, by thick wood fiber powder at sodium chlorite solution, glacial acetic acid solution
It manages, removes lignin under heating condition, obtain holocellulose, by holocellulose sodium hydroxide solution heat-insulation soaking, filtering point
From purifying cellulose is obtained, purifying cellulose is configured to water slurry, is ultrasonically treated, wooden nano-cellulose is made, by silicon
Colloidal sol, salpeter solution and absolute ethyl alcohol are mixed to get mixed liquor, then to being dripped in the mixture of normal heptane, n-butanol and sucrose ester
Add mixed liquor and ammonium hydroxide, be separated by filtration to obtain filter cake after being stirred to react, finally will obtain gel micro-ball after Washing of Filter Cake, with positive silicon
Acetoacetic ester is prepared to obtain reinforcing agent with absolute ethyl alcohol, and CO is put into after gel micro-ball is handled with reinforcing agent2Supercritical drying drying system
In be dried to obtain enhancing aeroge, then obtain the enhanced charcoal-aero gel of Ludox through charing, raw material of the present invention is natural timber,
The toxic chemicals such as phenol, hexamethylenetetramine and acetonitrile are not used, using chlorite oxidation's lignocellulosic, removing is wooden
Element is then sonicated dispersion and obtains the gel with Minute pores, utilizes the affine performance of Ludox and fiber, reinforcing fiber hole
Gap structure, to make the intensity of charcoal-aero gel be improved；
（2）The present invention has higher crystallinity and draw ratio, wooden Nanowire using gel made from wooden nano-cellulose
When dimension element is dispersed in water, three-dimensional net structure can be formed by interfibrous hydrogen bond and long stapled entanglement, is stablized
Hydrogel, fiber provide aeroge stabilization network skeleton, improve the intensity and film amount of aeroge, aeroge made to be answered
Power impact will not fragmentation, Ludox is not aerogel microball material in the present invention, and Ludox is aqueous when aerogel microball formation
Under the diffusion of solvent, into inside aerogel microball, the hydrogen atom structure of oxygen atom and cellulose aerogels microballoon in silica
At hydrogen bond, finally hydrogen bond makes the radius of aerogel microball reduce in single aerogel microball after carbonizing ablation, multiple
Between aerogel microball, hole reduces between making microballoon, but in general, microballoon is finer and close in the charcoal-aero gel of unit volume, increases
Porosity achievees the effect that improve charcoal-aero gel toughness, application prospect to make the stress dispersion effect of aeroge get a promotion
It is wide.
Specific implementation mode
It takes 200~300g poplars to be put into pulverizer, crushes 1~2h, cross 200 mesh standard sieves, obtain wooden powder, weigh
100~150g wooden powders are placed in Soxhlet extractor, are that 2 ︰ 1 are mixed to get benzene by volume at normal temperatures by benzyl carbinol and water
Ethanol solution, then 300~400mL benzyl carbinol solution is poured into Soxhlet extractor, 5~10h, removing are extracted at 80~90 DEG C
After extract, thick wood fiber powder is obtained；Thick wood fiber powder is put into beaker, 50~60mL mass fractions are added into beaker is
20% sodium chlorite solution, the glacial acetic acid solution for being 98% with mass fraction adjusts the pH to 4~5 of solution, in 75~80 DEG C of items
5~7h of isothermal holding under part, repeats aforesaid operations 3~5 times, removes lignin, obtains holocellulose；With 120~150mL mass
The sodium hydroxide solution that score is 20% impregnates holocellulose, 2~3h of heat-insulation soaking, filtering removal under the conditions of 90~100 DEG C
Filtrate obtains purifying cellulose, and purifying cellulose is made into the water slurry that mass fraction is 10~20%, is placed in ultrasonic wave plant
30~45min is handled with the power ultrasonic of 1200~1500W in cell disruptor, control supersonic frequency is 30~35kHz, is made
Wooden nano-cellulose；It counts in parts by weight, the Ludox for being 25% by 10~15 parts of mass fractions, 4~6 parts of mass fractions
It is added in beaker for 5% salpeter solution and 16~20 parts of absolute ethyl alcohol mixing, stirs 15~20min, obtain mixed liquor, then
100~110 portions of normal heptanes, 4~6 parts of n-butanols and 0.1~0.3 part of sucrose ester is added to three-necked flask；By mixed liquor constant pressure
Dropping funel is added dropwise to the drop rate of 3~5mL/min in three-necked flask, while starting blender, with 100~120r/min
Rotating speed stir 30~45min, the ammonium hydroxide that 4~5 parts of mass fractions are 5% is added dropwise and adds 30~40 parts of wooden nanofiber
Element is stirred to react 10~15min, the substance in filter flask, and removal filtrate obtains filter cake；Filter cake is washed 3~5 with acetone
It is secondary, gel micro-ball is obtained, under the conditions of 60~80 DEG C, is mixed to get in mass ratio for 1 ︰ 3 with absolute ethyl alcohol with ethyl orthosilicate
Reinforcing agent is put into CO after gel micro-ball is impregnated 3~5h with reinforcing agent2In supercritical drying drying system dry 20 at 70~80 DEG C
~for 24 hours, enhanced aeroge is obtained, enhanced aeroge is put into retort and is carbonized, it is nitrogen to control in retort
Or argon gas atmosphere, carbonization temperature are 600~1200 DEG C, carbonization time is 2~8h, obtains the enhanced charcoal-aero gel of Ludox.
It takes 200g poplars to be put into pulverizer, crushes 1h, cross 200 mesh standard sieves, obtain wooden powder, it is wooden to weigh 100g
Powder is placed in Soxhlet extractor, benzyl carbinol and water is mixed to get benzyl carbinol solution for 2 ︰ 1 by volume at normal temperatures, then will
300mL benzyl carbinol solution pours into Soxhlet extractor, and 5h is extracted at 80 DEG C, after removing extract, obtains thick wood fiber powder；It will
Thick wood fiber powder is put into beaker, and the sodium chlorite solution that 50mL mass fractions are 20% is added into beaker, is with mass fraction
98% glacial acetic acid solution adjusts pH to 4, isothermal holding 5h under the conditions of 75 DEG C of solution, repeats aforesaid operations 3 times, removing wood
Quality obtains holocellulose；The sodium hydroxide solution for being 20% with 120mL mass fractions, impregnates comprehensive fiber under the conditions of 90 DEG C
Element, heat-insulation soaking 2h, filtering removal filtrate obtain purifying cellulose, and purifying cellulose, which is made into the water that mass fraction is 10%, to be hanged
Supernatant liquid, is placed in ultrasonic wave plant cell pulverizer the power ultrasonic processing 30min with 1200W, and control supersonic frequency is
Wooden nano-cellulose is made in 30kHz；It counts in parts by weight, the Ludox for being 25% by 10 parts of mass fractions, 4 parts of quality point
Number is added for 5% salpeter solution and 16 parts of absolute ethyl alcohol mixing in beaker, stirs 15min, mixed liquor is obtained, then to three mouthfuls
100 portions of normal heptanes, 4 parts of n-butanols and 0.1~0.3 part of sucrose ester is added in flask；By mixed liquor constant pressure funnel with 3mL/
The drop rate of min is added dropwise in three-necked flask, while starting blender, is stirred 30min with the rotating speed of 100r/min, is added dropwise 4
The wooden nano-cellulose of 30 parts of ammonium hydroxide and addition that part mass fraction is 5%, is stirred to react 10min, the object in filter flask
Matter, removal filtrate obtain filter cake；Filter cake is washed 3 times with acetone, obtains gel micro-ball, under the conditions of 60 DEG C, with positive silicic acid second
Ester is that 1 ︰ 3 is mixed to get reinforcing agent in mass ratio with absolute ethyl alcohol, and CO is put into after gel micro-ball is impregnated 3h with reinforcing agent2It is super to face
20h is dried in boundary's drying system at 70 DEG C, enhanced aeroge is obtained, enhanced aeroge is put into retort and carries out charcoal
Change, it is nitrogen or argon gas atmosphere to control in retort, and carbonization temperature is 600 DEG C, and it is enhanced to obtain Ludox by carbonization time 2h
Charcoal-aero gel.
It takes 250g poplars to be put into pulverizer, crushes 1.5h, cross 200 mesh standard sieves, obtain wooden powder, weigh 125g wood
Matter powder is placed in Soxhlet extractor, and benzyl carbinol and water are mixed to get benzyl carbinol solution for 2 ︰ 1 by volume at normal temperatures, then
350mL benzyl carbinol solution is poured into Soxhlet extractor, 7h is extracted at 85 DEG C, after removing extract, obtains thick wood fiber powder；
Thick wood fiber powder is put into beaker, the sodium chlorite solution that 55mL mass fractions are 20% is added into beaker, uses mass fraction
PH to 4.5, isothermal holding 6h under the conditions of 77 DEG C of solution are adjusted for 98% glacial acetic acid solution, repeats aforesaid operations 4 times, is taken off
Except lignin, holocellulose is obtained；The sodium hydroxide solution for being 20% with 135mL mass fractions, impregnates comprehensive fibre under the conditions of 95 DEG C
Dimension element, heat-insulation soaking 2.5h, filtering removal filtrate obtain purifying cellulose, and it is 15% that purifying cellulose, which is made into mass fraction,
Water slurry, is placed in ultrasonic wave plant cell pulverizer the power ultrasonic processing 38min with 1250W, and control supersonic frequency is
Wooden nano-cellulose is made in 33kHz；It counts in parts by weight, the Ludox for being 25% by 13 parts of mass fractions, 5 parts of quality point
Number is added for 5% salpeter solution and 18 parts of absolute ethyl alcohol mixing in beaker, stirs 17min, mixed liquor is obtained, then to three mouthfuls
105 portions of normal heptanes, 5 parts of n-butanols and 0.2 part of sucrose ester is added in flask；By mixed liquor constant pressure funnel with 4mL/min's
Drop rate is added dropwise in three-necked flask, while starting blender, stirs 38min with the rotating speed of 110r/min, 4.5 parts of matter are added dropwise
The ammonium hydroxide that score is 5% and the wooden nano-cellulose of 35 parts of addition are measured, is stirred to react 13min, the substance in filter flask is gone
Except filtrate obtains filter cake；Filter cake is washed 4 times with acetone, gel micro-ball is obtained, under the conditions of 70 DEG C, with ethyl orthosilicate and nothing
Water-ethanol is that 1 ︰ 3 is mixed to get reinforcing agent in mass ratio, and CO is put into after gel micro-ball is impregnated 4h with reinforcing agent2Supercritical drying
22h is dried in system at 75 DEG C, enhanced aeroge is obtained, enhanced aeroge is put into retort and is carbonized, is controlled
It is nitrogen or argon gas atmosphere in retort processed, carbonization temperature is 900 DEG C, carbonization time 5h, obtains the enhanced charcoal gas of Ludox
Gel.
It takes 300g poplars to be put into pulverizer, crushes 2h, cross 200 mesh standard sieves, obtain wooden powder, it is wooden to weigh 150g
Powder is placed in Soxhlet extractor, benzyl carbinol and water is mixed to get benzyl carbinol solution for 2 ︰ 1 by volume at normal temperatures, then will
400mL benzyl carbinol solution pours into Soxhlet extractor, and 10h is extracted at 90 DEG C, after removing extract, obtains thick wood fiber powder；
Thick wood fiber powder is put into beaker, the sodium chlorite solution that 60mL mass fractions are 20% is added into beaker, uses mass fraction
PH to 5, isothermal holding 7h under the conditions of 80 DEG C of solution are adjusted for 98% glacial acetic acid solution, repeats aforesaid operations 5 times, removing
Lignin obtains holocellulose；The sodium hydroxide solution for being 20% with 150mL mass fractions, impregnates comprehensive fibre under the conditions of 100 DEG C
Dimension element, heat-insulation soaking 3h, filtering removal filtrate obtain purifying cellulose, purifying cellulose are made into the water that mass fraction is 20%
Suspension, is placed in ultrasonic wave plant cell pulverizer the power ultrasonic processing 45min with 1500W, and control supersonic frequency is
Wooden nano-cellulose is made in 35kHz；It counts in parts by weight, the Ludox for being 25% by 15 parts of mass fractions, 6 parts of quality point
Number is added for 5% salpeter solution and 20 parts of absolute ethyl alcohol mixing in beaker, stirs 20min, mixed liquor is obtained, then to three mouthfuls
110 portions of normal heptanes, 6 parts of n-butanols and 0.3 part of sucrose ester is added in flask；By mixed liquor constant pressure funnel with 5mL/min's
Drop rate is added dropwise in three-necked flask, while starting blender, stirs 45min with the rotating speed of 120r/min, 5 parts of quality are added dropwise
The wooden nano-cellulose of 40 parts of ammonium hydroxide and addition that score is 5%, is stirred to react 15min, the substance in filter flask, removal
Filtrate obtains filter cake；Filter cake is washed 5 times with acetone, obtains gel micro-ball, under the conditions of 80 DEG C, with ethyl orthosilicate with it is anhydrous
Ethyl alcohol is that 1 ︰ 3 is mixed to get reinforcing agent in mass ratio, and CO is put into after gel micro-ball is impregnated 5h with reinforcing agent2Supercritical drying system
It is dry at 80 DEG C in system to obtain enhanced aeroge for 24 hours, enhanced aeroge is put into retort and is carbonized, it controls
It is nitrogen or argon gas atmosphere in retort, carbonization temperature is 1200 DEG C, carbonization time 8h, obtains the enhanced charcoal airsetting of Ludox
Glue.
The charcoal-aero gel that comparative example is produced with company of Shenzhen is molten using silicon to produced by the present invention as a comparison case
Charcoal-aero gel in the enhanced charcoal-aero gel of glue and comparative example is detected, and testing result is as shown in table 1：
Thermal conductivity is tested
Reference《Technology of Steady State Thermal Resistance of Thermal Insulating Material and measurement heat-flow meter method in relation to characteristic》（GB/T10295-2008）It is tested.
1 performance measurement result of table
| Test event | Example 1 | Example 2 | Example 3 | Comparative example |
| Density（g/cm3） | 0.28 | 0.27 | 0.25 | 0.35 |
| Tensile strength（MPa） | 0.33 | 0.33 | 0.35 | 0.14 |
| Compressive strength（MPa） | 96 | 101 | 104 | 53 |
| Bending strength（MPa） | 32.1 | 33.9 | 34.6 | 22.0 |
| Compression strength（MPa） | 3.06 | 3.22 | 3.37 | 1.51 |
| Thermal coefficient W/（m·K） | 0.021 | 0.020 | 0.019 | 0.038 |
| Specific surface area（m2/g） | 882 | 871 | 864 | 846 |
| Porosity（%） | 94 | 94 | 96 | 86 |
According to data in table 1 it is found that produced by the present invention utilize the enhanced charcoal-aero gel of Ludox, there is good integrality,
Its density is relatively low, and heat conductivility is good, and intensity is high, good mechanical performance, and raw materials are natural timber, and benzene is not used
The toxic chemicals such as phenol, hexamethylenetetramine and acetonitrile, therefore not will produce any harmful toxic matter, before there is wide use
Scape.
Claims (7)
1. a kind of preparation method of the enhanced charcoal-aero gel of Ludox, it is characterised in that specifically preparation process is：
（1）It takes 200~300g poplars to be put into pulverizer, crushes, cross standard screen, obtain wooden powder, weigh 100~150g wood
Matter powder is placed in Soxhlet extractor, and benzyl carbinol and water are mixed to get benzyl carbinol solution at normal temperatures, then by 300~400mL
Benzyl carbinol solution pours into Soxhlet extractor, and extracting obtains thick wood fiber powder after removing extract；
（2）Thick wood fiber powder is put into beaker, 50~60mL sodium chlorite solutions are added into beaker, with glacial acetic acid solution tune
The pH of solution is saved, isothermal holding repeats aforesaid operations 3~5 times, removes lignin, obtains holocellulose；
（3）Holocellulose is impregnated under the conditions of 90~100 DEG C with 120~150mL sodium hydroxide solutions, heat-insulation soaking filters off
Except filtrate obtains purifying cellulose, purifying cellulose is made into water slurry, is placed in ultrasonic wave plant cell pulverizer ultrasonic
Wooden nano-cellulose is made in processing；
（4）It counts in parts by weight, by 10~15 parts of Ludox, 4~6 parts of salpeter solutions and 16~20 parts of absolute ethyl alcohol mixing add
Enter in beaker, stir, obtain mixed liquor, 100~110 portions of normal heptanes, 4~6 parts of n-butanols and 0.1 are added then to three-necked flask
~0.3 part of sucrose ester；
（5）Mixed liquor is added dropwise to constant pressure funnel in three-necked flask, while starting blender stirring, 4~5 parts of ammonia are added dropwise
Water and the wooden nano-cellulose of 30~40 parts of addition, are stirred to react, the substance in filter flask, and removal filtrate obtains filter cake；
（6）Filter cake is washed 3~5 times with acetone, gel micro-ball is obtained, under the conditions of 60~80 DEG C, with ethyl orthosilicate and nothing
Water-ethanol is mixed to get reinforcing agent, and CO is put into after gel micro-ball is impregnated with reinforcing agent2It is dry in supercritical drying drying system, it obtains
Enhanced aeroge is put into retort and is carbonized by enhanced aeroge, obtains the enhanced charcoal-aero gel of Ludox.
2. a kind of preparation method of the enhanced charcoal-aero gel of Ludox according to claim 1, it is characterised in that：Step
（1）The grinding time is 1~2h, and be sieved specification is 200 mesh, and mixed volume ratio is 2 ︰ 1 to benzyl carbinol at normal temperatures with water,
Extraction temperature is 80~90 DEG C, and the time is 5~10h.
3. a kind of preparation method of the enhanced charcoal-aero gel of Ludox according to claim 1, it is characterised in that：Step
（2）The mass fraction of the sodium chlorite solution is 20%, and glacial acetic acid solution mass fraction is 98%, and glacial acetic acid solution adjusts molten
The pH of liquid is 4~5, and the isothermal holding time is 5~7h.
4. a kind of preparation method of the enhanced charcoal-aero gel of Ludox according to claim 1, it is characterised in that：Step
（3）The mass fraction of the sodium hydroxide solution is 20%, and the heat-insulation soaking time is 2~3h, and the mass fraction of water slurry is
10~20%, the power of supersound process is 1200~1500W, and ultrasonic time is 30~45min, control supersonic frequency is 30~
35kHz。
5. a kind of preparation method of the enhanced charcoal-aero gel of Ludox according to claim 1, it is characterised in that：Step
（4）The mass fraction of the Ludox is 25%, and the mass fraction of salpeter solution is 5%, and mixing time is 15~20min.
6. a kind of preparation method of the enhanced charcoal-aero gel of Ludox according to claim 1, it is characterised in that：Step
（5）The constant pressure funnel drop rate is 3~5mL/min, and speed of agitator is 100~120r/min, and mixing time is
The mass fraction of 30~45min, ammonium hydroxide are 5%, and it is 10~15min to be stirred to react the time.
7. a kind of preparation method of the enhanced charcoal-aero gel of Ludox according to claim 1, it is characterised in that：Step
（6）The ethyl orthosilicate and absolute ethyl alcohol mixing quality ratio are 1 ︰ 3, the time that gel micro-ball reinforcing agent impregnates is 3~
5h, supercritical drying temperature be 70~80 DEG C, drying time be 20~for 24 hours, control retort in be nitrogen or argon gas atmosphere, charcoal
It is 600~1200 DEG C to change temperature, and carbonization time is 2~8h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810289595.5A CN108298519A (en) | 2018-03-30 | 2018-03-30 | A kind of preparation method using the enhanced charcoal-aero gel of Ludox |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810289595.5A CN108298519A (en) | 2018-03-30 | 2018-03-30 | A kind of preparation method using the enhanced charcoal-aero gel of Ludox |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108298519A true CN108298519A (en) | 2018-07-20 |
Family
ID=62846961
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810289595.5A Pending CN108298519A (en) | 2018-03-30 | 2018-03-30 | A kind of preparation method using the enhanced charcoal-aero gel of Ludox |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108298519A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108862239A (en) * | 2018-09-28 | 2018-11-23 | 陈太师 | A kind of preparation method of high tenacity charcoal-aero gel |
| CN109762209A (en) * | 2018-12-21 | 2019-05-17 | 珠海水丝新材料有限公司 | A kind of production method of the gel sponge membrane body of built-in long fibre skeleton |
| CN111574210A (en) * | 2020-05-20 | 2020-08-25 | 佛山科学技术学院 | Nano porous heat insulation material |
| CN113310607A (en) * | 2021-06-24 | 2021-08-27 | 华中科技大学 | Flexible touch sensing array, preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104609394A (en) * | 2015-02-13 | 2015-05-13 | 东北林业大学 | Preparation method of biomass nano cellulose carbon aerogel |
| CN105502346A (en) * | 2016-01-27 | 2016-04-20 | 中国林业科学研究院木材工业研究所 | Carbon aerogel prepared from chitin aerogel and preparation method thereof |
| CN107686562A (en) * | 2017-09-25 | 2018-02-13 | 常州新区金利宝塑料制品有限公司 | A kind of preparation method of cellulose aerogels microballoon |
-
2018
- 2018-03-30 CN CN201810289595.5A patent/CN108298519A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104609394A (en) * | 2015-02-13 | 2015-05-13 | 东北林业大学 | Preparation method of biomass nano cellulose carbon aerogel |
| CN105502346A (en) * | 2016-01-27 | 2016-04-20 | 中国林业科学研究院木材工业研究所 | Carbon aerogel prepared from chitin aerogel and preparation method thereof |
| CN107686562A (en) * | 2017-09-25 | 2018-02-13 | 常州新区金利宝塑料制品有限公司 | A kind of preparation method of cellulose aerogels microballoon |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108862239A (en) * | 2018-09-28 | 2018-11-23 | 陈太师 | A kind of preparation method of high tenacity charcoal-aero gel |
| CN109762209A (en) * | 2018-12-21 | 2019-05-17 | 珠海水丝新材料有限公司 | A kind of production method of the gel sponge membrane body of built-in long fibre skeleton |
| CN111574210A (en) * | 2020-05-20 | 2020-08-25 | 佛山科学技术学院 | Nano porous heat insulation material |
| CN113310607A (en) * | 2021-06-24 | 2021-08-27 | 华中科技大学 | Flexible touch sensing array, preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108298519A (en) | A kind of preparation method using the enhanced charcoal-aero gel of Ludox | |
| Lu et al. | Fabrication of mesoporous lignocellulose aerogels from wood via cyclic liquid nitrogen freezing–thawing in ionic liquid solution | |
| CN104448397B (en) | A kind of cellulose-silicon dioxide composite aerogel in-situ preparation method | |
| CN107686562A (en) | A kind of preparation method of cellulose aerogels microballoon | |
| CN109516458A (en) | A kind of biomass-based graded porous carbon and preparation method thereof | |
| CN105418052B (en) | A kind of preparation process of carbon nano-fiber combined oxidation silica aerogel | |
| CN102912686B (en) | Filter paper for air filter containing modified nano bamboo charcoal powder | |
| CN105600768B (en) | A kind of self-supporting porous carbon for electrode material for super capacitor and preparation method thereof | |
| CN107051339B (en) | Fiber composite toughened SiO2Aerogel and preparation method thereof | |
| CN105502346B (en) | A kind of carbon aerogels prepared using chitin aerogel and preparation method thereof | |
| CN106750550B (en) | A kind of fire retardant elastic nano-cellulose aerogel and preparation method thereof | |
| CN107840979B (en) | A kind of preparation method of crosslinking nano cellulose/hexagonal boron nitride nanosheet composite membrane | |
| CN108704624A (en) | A kind of preparation method of photocatalytic activity adsorbent | |
| CN102877375A (en) | Preparation method for modified kaolin-containing filter paper for air filter | |
| CN110078048A (en) | A kind of carbon aerogels natural gas adsorbent and its preparation method and application | |
| CN109534342A (en) | The preparation method of biomass super-activated carbon | |
| CN109954329A (en) | A kind of anti-haze filtering layer material of plant fiber self-supporting graphene and its preparation method and application | |
| CN108191451A (en) | A kind of high intensity, porous sound-absorbing material and preparation method thereof | |
| CN111944068A (en) | Biomass sponge and preparation method and application thereof | |
| CN115725111B (en) | Composite aerogel with broadband low-frequency sound absorption and heat insulation functions and preparation and application thereof | |
| JP2006225231A (en) | Activated carbon from chitinous matter as raw material and its manufacturing method | |
| CN107298821A (en) | A kind of preparation method of highly hygroscopic speed hygroscopic material | |
| CN104005273A (en) | Zeolite molecular sieve supported air filter paper and making method thereof | |
| CN109092246A (en) | A kind of preparation method of porous carbon adsorbing material | |
| CN110407208A (en) | A kind of preparation method of mesoporous graphene-based charcoal-aero gel |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180720 |