CN110282995A - A kind of porous silicon carbide wood ceramic preparation based on cellulose aerogels template - Google Patents
A kind of porous silicon carbide wood ceramic preparation based on cellulose aerogels template Download PDFInfo
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Abstract
The present invention provides a kind of porous silicon carbide wood ceramic preparation based on cellulose aerogels template, Ba Ersha lignose aeroge to remove part hemicellulose and lignin prepares porous silicon carbide wood ceramics by ceramic forerunner dipping-cracking technology as template.This method is by destroying part wood cell wall construction, open cell corner, through part pit membrane, more pore structures have been built inside template, to improve template to the assimilation effect of ceramics precursor liquid solution, the porosity for improving porous silicon carbide wood ceramics under prior art is low, the problem of pore structure degree of communication difference, and the functionalized application for porous silicon carbide wood ceramics lays the foundation.
Description
Technical field
The present invention relates to a kind of porous silicon carbide wood ceramic preparation based on cellulose aerogels template, belongs to biology
The technical field of material preparation aspect.
Background technique
Silicon carbide woodceramics are will to plant source biomass material to be introduced into the preparation process of pure silicon carbide ceramics, merge silicon carbide
The spies such as the excellent physicals chemical properties such as high-intensitive, corrosion-resistant, anti-thermal shock of ceramics itself and biological material are renewable, source is wide
Point, a kind of obtained novel biomass base silicon carbide composite material.Porous silicon carbide wood ceramics are as electrode material, dedusting
The fields such as filter, insulation medium have broad application prospects, but at present prepare porous silicon carbide wood ceramics method mainly with
Solid wood is starting material, is obtained by the organic precursor Polycarbosilane (PCS) of impregnated carbon SiClx ceramics, then through Pintsch process
Porous silicon carbide wood ceramics.It is this that porous silicon carbide wood ceramic preparation face is prepared directly as bionical template with solid wood
Face the problems such as wood microstructure variability is big, there are anisotropy.Finished form is simple, size is less than normal, and porosity is low, Kong Jie
Structure degree of communication is poor, is unfavorable for further developing and using, thus needs to improve the preparation method of silicon carbide woodceramics.
The main composition of timber is cellulose, hemicellulose and lignin.Cellulose assigns timber tensile strength, structure
At the basic skeleton structure of timber, hemicellulose and lignin are filled in cellulose skeleton as base matter, by fiber
The fibril gluing of element composition is together.If, can using chemical means by hemicellulose a part of in timber and delignification
To obtain the cellulose aerogels with three-dimensional porous structure.Since chemical treatment is stripped of Timber sections hemicellulose and wooden
Element, wood cell wall is destructurized, and cell corner is opened, and part pit membrane is run through, therefore this cellulose aerogels matter
Amount is light, and porosity is high, and pore connectivity is good, while having certain absorbability.These characteristics based on cellulose aerogels,
Based on ceramic forerunner dipping-cracking technology, use cellulose aerogels as the bionical mould of porous silicon carbide wood ceramics
Plate wherein by PCS solution negative pressure impregnation, and then can sinter porous silicon carbide wood ceramics into.Compared to existing with solid wood
The permeability of template is improved first using cellulose aerogels as template for the method for template, so that precursor solution more holds
Easily it is sufficiently impregnated；Secondly, the porosity and pore connectivity of cellulose aerogels template are higher, therefore can be effectively improved porous
The porosity of silicon carbide woodceramics is low, the problem of pore structure degree of communication difference, and the functionalized application for porous silicon carbide wood ceramics is established
Fixed basis.
Summary of the invention
The purpose of the present invention is intended in view of the deficiencies of the prior art, provide a kind of more using cellulose aerogels as template preparation
The method of hole silicon carbide wood ceramics.The preparation method simple process, easily controllable, low energy consumption, by chemical treatment removing part half
Bionical template of the Ba Ersha lignose aeroge of cellulose and lignin as porous silicon carbide wood ceramics, helps to improve
The porosity of porous silicon carbide wood ceramics is low, and the problem of pore structure degree of communication difference improves the quality of porous silicon carbide wood ceramics
With performance.The technical scheme adopted by the invention is as follows: a kind of porous silicon carbide wood ceramic system based on cellulose aerogels template
Preparation Method, the specific steps of which are as follows:
(1) appropriate NaOH and Na is weighed2SO3Be dissolved in deionized water configure mixed solution it is spare, in mixed solution NaOH with
Na2SO3Substance withdrawl syndrome be respectively 2.5mol/L and 0.4mol/L.
(2) Ba Ersha wooden (latin name Ochroma lagopus) is processed as the cube of certain size, be wrapped in medical
In absorbent gauze, boiling is immersed in above-mentioned mixed solution for a period of time.
(3) wooden unit after boiling is taken out together with gauze, after being washed with deionized water, is placed in the H of 30wt%2O2Water
Continue boiling for a period of time in solution.
(4) by treated, wooden unit takes out together with gauze, is placed in boiling 3h in deionized water, removes remaining H2O2,
It is freeze-dried the gauze for removing package for 24 hours later, obtains cellulose aerogels.
(5) appropriate Polycarbosilane solid powder is taken, is dissolved using dimethylbenzene as solvent, is configured to the ceramic slurry of 40wt%
Material.Bulk fibers element aeroge is cut into suitable dimension, is put into ceramic slurry and is taken out after vacuum impregnation 12h, it is appropriate to heat
Xylene solvent is removed, the ceramic pre-sintered body of porous silicon carbide wood is obtained.
(6) the ceramic pre-sintered body of porous silicon carbide wood is put into graphite crucible, is placed in atmosphere sintering in high temperature sintering furnace,
Furnace cooling obtains porous silicon carbide wood ceramics.
Preferably, in the step (1), the mixed liquor volume of configuration should be the 20- of Ba Ersha wood volume to be processed
30 times.
Preferably, in the step (2), the side length of Ba Ersha cube wooden unit should be controlled in 10-20mm, molten with mixing
The time of liquid boiling is 20-24h.
Preferably, in the step (3), H is used2O2The time of aqueous solution boiling is 8-10h.
Preferably, in the step (5), Polycarbosilane used should be the powder of 100 mesh or more to promote to dissolve, and slurry is matched
The process of setting, which should use magnetic agitation to mix and pay attention to sealing in container, prevents dimethylbenzene from volatilizing, and Monolithic aerogel should be cut into thickness
Sheet no more than 3mm, vacuum-impregnated vacuum degree should be 0.08MPa.
Preferably, in the step (6), sintering temperature is 1400-1500 DEG C, and overall process leads to argon gas protection, heating rate
5-15 DEG C/min, stop heating, sample furnace cooling after keeping the temperature 1h.
Compared with prior art, the present invention has the following advantages and effects:
1, using cellulose aerogels as porous silicon carbide wood ceramics bionical template, impregnate with presoma-crack work
Skill prepares porous silicon carbide wood ceramics, and compared with the existing direct method using solid wood for template, template is to ceramics precursor
The permeability of liquid solution greatly improves, and required dip time is shorter, and dipping is more abundant, therefore has in ceramic product to mechanical strength
Dysgenic agraphitic carbon content is less.
2, there are a large amount of visible and sightless pore structures compared to solid wood, in cellulose aerogels template, this
Some holes gap structure can be replicated by presoma dipping-cracking technology, the porosity and porosity communication of the porous wooden ceramic product of gained
Degree greatly improves, and the porosity for effectively improving porous silicon carbide wood ceramics under prior art is low, and pore structure degree of communication difference is asked
Topic, the functionalized application for porous silicon carbide wood ceramics lay the foundation.
3, the preparation method process is simple, and simple process is easily controllable, and low energy consumption, have good development prospect and into
One step deeply expands the value of research.
Specific embodiment
Below with reference to specific implementation example, the present invention is described in detail:
Embodiment 1
(1) 40g NaOH and 20.16g Na are taken2SO3It is spare to be carefully dissolved in configuration mixed solution in 400ml deionized water.
(2) by 20cm3Ba Er China fir is processed into the cube wooden unit of 20mm square, is wrapped in medical absorbent cotton/gauze, leaching
Enter boiling 20h in above-mentioned mixed solution.
(3) wooden unit after boiling is taken out together with gauze, after being washed with deionized water, is placed in the H of 30wt%2O2Water
Continue boiling 8h in solution.The ceramic slurry for taking appropriate poplar wood powder dipping equal quality, stands for 24 hours after mixing well.
(4) by treated, wooden unit takes out together with gauze, is placed in boiling 3h in deionized water, removes remaining H2O2,
It is freeze-dried the gauze for removing package for 24 hours later, obtains cellulose aerogels.
(6) 30g Polycarbosilane solid is ground into 100 mesh powder, is dissolved using dimethylbenzene as solvent, is configured to 40wt%'s
Ceramic slurry.The square piece of bulk fibers element aeroge cutting 2mm thickness is put into ceramic slurry with 0.08MPa vacuum degree dipping
It is taken out after 12h, appropriate heating removes xylene solvent, obtains the ceramic pre-sintered body of porous silicon carbide wood.
(6) by porous silicon carbide wood ceramics, pre-sintered body is smooth is put into graphite crucible, is placed in sintering furnace with 1400 DEG C
Ar-sintering, 5 DEG C/min of heating rate keep the temperature 1h, and sample furnace cooling obtains porous silicon carbide wood ceramics.
Embodiment 2
(1) 80g NaOH and 40.32g Na are taken2SO3It is spare to be carefully dissolved in configuration mixed solution in 800ml deionized water.
(2) by 40cm3Ba Er China fir is processed into the cube wooden unit of 15mm square, immerses boiling in above-mentioned mixed solution
24h。
(3) wooden unit after boiling is taken out together with gauze, after being washed with deionized water, is placed in the H of 30wt%2O2Water
Continue boiling 10h in solution.The ceramic slurry for taking appropriate poplar wood powder dipping equal quality, stands for 24 hours after mixing well.
(4) by treated, wooden unit takes out together with gauze, is placed in boiling 3h in deionized water, removes remaining H2O2,
It is freeze-dried the gauze for removing package for 24 hours later, obtains cellulose aerogels.
(6) 60g Polycarbosilane solid is ground into 100 mesh powder, is dissolved using dimethylbenzene as solvent, is configured to 40wt%'s
Ceramic slurry.The square piece of bulk fibers element aeroge cutting 3mm thickness is put into ceramic slurry with 0.08MPa vacuum degree dipping
It is taken out after 12h, appropriate heating removes xylene solvent, obtains the ceramic pre-sintered body of porous silicon carbide wood.
(6) by porous silicon carbide wood ceramics, pre-sintered body is smooth is put into graphite crucible, is placed in sintering furnace with 1500 DEG C
Ar-sintering, 10 DEG C/min of heating rate keep the temperature 1h, and sample furnace cooling obtains porous silicon carbide wood ceramics.
Claims (6)
1. a kind of porous silicon carbide wood ceramic preparation based on cellulose aerogels template, which is characterized in that including as follows
Several steps:
(1) appropriate NaOH and Na is weighed2SO3Be dissolved in deionized water configure mixed solution it is spare, in mixed solution NaOH with
Na2SO3Substance withdrawl syndrome be respectively 2.5mol/L and 0.4mol/L；
(2) Ba Ersha wooden (latin name Ochroma lagopus) is processed as the cube of certain size, is wrapped in medical degreasing
In gauze, boiling is immersed in above-mentioned mixed solution for a period of time；
(3) wooden unit after boiling is taken out together with gauze, after being washed with deionized water, is placed in the H of 30wt%2O2Aqueous solution
Middle continuation boiling is for a period of time；
(4) by treated, wooden unit takes out together with gauze, is placed in boiling 3h in deionized water, removes remaining H2O2, later
Freeze-drying for 24 hours, removes the gauze of package, obtains cellulose aerogels；
(5) appropriate Polycarbosilane solid powder is taken, is dissolved using dimethylbenzene as solvent, is configured to the ceramic slurry of 40wt%, it will
Bulk fibers element aeroge is cut into suitable dimension, is put into ceramic slurry and takes out after vacuum impregnation 12h, and appropriate heating removes two
Toluene solvant obtains the ceramic pre-sintered body of porous silicon carbide wood；
(6) the ceramic pre-sintered body of porous silicon carbide wood is put into graphite crucible, atmosphere sintering in high temperature sintering furnace is placed in, with furnace
It is cooling to obtain porous silicon carbide wood ceramics.
2. a kind of porous silicon carbide wood ceramic preparation based on cellulose aerogels template according to claim 1,
It is characterized in that, the mixed liquor volume of configuration should be 20-30 times of Ba Ersha wood volume to be processed in the step (1).
3. a kind of porous silicon carbide wood ceramic preparation based on cellulose aerogels template according to claim 1,
It is characterized in that, the side length of Ba Ersha cube wooden unit should be controlled in 10-20mm in the step (2), steamed with mixed solution
The time boiled is 20-24h.
4. a kind of preparation method of the wooden ceramic body of silicon carbide according to claim 1, which is characterized in that the step
(3) in, H is used2O2The time of aqueous solution boiling is 8-10h.
5. a kind of porous silicon carbide wood ceramic preparation based on cellulose aerogels template according to claim 1,
It is characterized in that, Polycarbosilane used should be the powder of 100 mesh or more to promote to dissolve, and slurry configured in the step (5)
Journey, which should use magnetic agitation to mix and pay attention to sealing in container, prevents dimethylbenzene from volatilizing, and Monolithic aerogel should be cut into thickness and not surpass
The sheet of 3mm is crossed, vacuum-impregnated vacuum degree should be 0.08MPa.
6. a kind of porous silicon carbide wood ceramic preparation based on cellulose aerogels template according to claim 1,
It is characterized in that, sintering temperature is 1400-1500 DEG C in the step (6), overall process leads to argon gas protection, heating rate 5-15
DEG C/min, stop heating, sample furnace cooling after keeping the temperature 1h.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112142492A (en) * | 2020-09-27 | 2020-12-29 | 南京工业职业技术大学 | Novel method for preparing piezoelectric ferroelectric composite material |
| CN112499612A (en) * | 2020-12-23 | 2021-03-16 | 北京林业大学 | Silicon carbide ceramic derived carbon material with wood hierarchical pore structure and preparation method thereof |
| CN113019015A (en) * | 2019-12-24 | 2021-06-25 | 东北林业大学 | Cake-shaped wood fiber ceramic engine air filter element |
| CN113046030A (en) * | 2021-02-04 | 2021-06-29 | 上海大学 | Preparation method of delignified balsawood/phase-change composite material |
| CN113200543A (en) * | 2021-06-18 | 2021-08-03 | 南京林业大学 | Method for preparing activated carbon precursor by intervention of biomass oil |
| CN113788701A (en) * | 2021-09-07 | 2021-12-14 | 华中科技大学 | Preparation method and product of 3D printing lignocellulose derived silicon carbide ceramic |
| CN113929100A (en) * | 2021-10-08 | 2022-01-14 | 西安交通大学 | Porous silicon carbide aerogel and preparation method based on natural wood |
| CN114854177A (en) * | 2022-04-26 | 2022-08-05 | 华南理工大学 | Nonlinear conductive epoxy resin composite material and preparation method and application thereof |
| CN115745655A (en) * | 2022-10-31 | 2023-03-07 | 南京航空航天大学 | Preparation method of porous silicon carbide ceramic material and preparation method of phase-change heat storage material of porous silicon carbide ceramic material |
| CN116580520A (en) * | 2023-07-14 | 2023-08-11 | 江苏恒力化纤股份有限公司 | Fire disaster early warning aerogel and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113019015A (en) * | 2019-12-24 | 2021-06-25 | 东北林业大学 | Cake-shaped wood fiber ceramic engine air filter element |
| CN112142492A (en) * | 2020-09-27 | 2020-12-29 | 南京工业职业技术大学 | Novel method for preparing piezoelectric ferroelectric composite material |
| CN112499612A (en) * | 2020-12-23 | 2021-03-16 | 北京林业大学 | Silicon carbide ceramic derived carbon material with wood hierarchical pore structure and preparation method thereof |
| CN113046030A (en) * | 2021-02-04 | 2021-06-29 | 上海大学 | Preparation method of delignified balsawood/phase-change composite material |
| CN113200543A (en) * | 2021-06-18 | 2021-08-03 | 南京林业大学 | Method for preparing activated carbon precursor by intervention of biomass oil |
| CN113788701A (en) * | 2021-09-07 | 2021-12-14 | 华中科技大学 | Preparation method and product of 3D printing lignocellulose derived silicon carbide ceramic |
| CN113929100A (en) * | 2021-10-08 | 2022-01-14 | 西安交通大学 | Porous silicon carbide aerogel and preparation method based on natural wood |
| CN114854177A (en) * | 2022-04-26 | 2022-08-05 | 华南理工大学 | Nonlinear conductive epoxy resin composite material and preparation method and application thereof |
| CN114854177B (en) * | 2022-04-26 | 2022-12-16 | 华南理工大学 | Nonlinear conductive epoxy resin composite material and preparation method and application thereof |
| CN115745655A (en) * | 2022-10-31 | 2023-03-07 | 南京航空航天大学 | Preparation method of porous silicon carbide ceramic material and preparation method of phase-change heat storage material of porous silicon carbide ceramic material |
| CN116580520A (en) * | 2023-07-14 | 2023-08-11 | 江苏恒力化纤股份有限公司 | Fire disaster early warning aerogel and preparation method thereof |
| CN116580520B (en) * | 2023-07-14 | 2023-09-19 | 江苏恒力化纤股份有限公司 | Fire disaster early warning aerogel and preparation method thereof |
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Application publication date: 20190927 |