CN103833003A - Method for preparing larch based ordered mesoporous carbon by virtue of soft template - Google Patents
Method for preparing larch based ordered mesoporous carbon by virtue of soft template Download PDFInfo
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Abstract
The invention provides a method for preparing a larch based ordered mesoporous carbon by virtue of a soft template. The method is characterized by comprising the steps of by taking the larch dust as the raw material and phenol as the liquifier, liquifying the larch to obtain a larch liquid under an acidic condition, reacting the larch liquid with formaldehyde under an alkali condition to generate phenolic resin, selecting a block copolymer F127 as the soft template and reacting under the acidic condition to generate the intermediate phase of the larch based ordered mesoporous carbon, and under the condition of nitrogen protection, calcining the intermediate phase of the larch based ordered mesoporous carbon to obtain the product. The method is mainly characterized in that as the biomass larch is taken as the raw material, the raw material is abundant, and the resource is reutilized, which is advantageous for saving energy and reducing consumption, the larch based dust is decomposed by the liquifying method so that the internal structure of the larch based dust is easier to regulate and control, and moreover, the mild soft template agent, namely the block copolymer F127, is selected to achieve successful regulation and control of the ordered mesoporous carbon, and furthermore, the method has the advantages of low pollution and high yield.
Description
Affiliated technical field:
The present invention relates to biomass charcoal Material Field, particularly relate to a kind of preparation method of soft template method tamarack base ordered mesoporous carbon.
Background technology:
Porous carbon material receives much concern as a kind of novel charcoal material, can, according to its special pore texture and different microscopic appearances, be widely used in the fields such as fractionation by adsorption, diffusion, support of the catalyst, energy storage.Physical chemistry activation method, mixed with polymers charring, organic gel method and template synthesis are mainly passed through in the preparation of mesoporous carbon at present take coal tar, pitch, oil, polymkeric substance etc. as raw material.Ordered mesoporous carbon has periodic duct, large pore volume, large specific surface area, the concentrated advantage such as mesoporous distribution and adjustable aperture, is the desired separated material model of research fractionation by adsorption.Mesoporous carbon material can be made by catalytic activation method, organogel charring and template, but only has template just can obtain orderly pore structure.So far, to show to adopt segmented copolymer be that template is prepared ordered mesoporous carbon in existing a large amount of research.
The high value of Wooden Biomass resource transforms and efficient utilization research is more and more paid attention in recent years.Except traditional charcoal and gac, it is applied to high added value new carbon preparation field and has more limitation, reports at present less.Wood liquefiedly make solid-state timber macromolecules degradation, making wood conversion is alcohols, flammable oil or other compounds with particular functional group, not only can further control the internal structure of timber, further polymerization changes into the biomass-based high polymer material of resene of easy forming process.Therefore, selecting biomass is raw material, and preparing ordered mesoporous carbon material has important realistic meaning and using value.
United States Patent (USP) (US7910082B2) has been introduced with resol, and tetraethyl orthosilicate, tensio-active agent and the butanols of prehydrolysis are raw material, are mixed, are cross-linked, add thermosetting size homogeneous, disperse orderly order mesoporous silicon carbide.Be raw material because this method adopts tetraethyl orthosilicate, toxicity is higher, contaminate environment, and be difficult for large-scale production.
United States Patent (USP) (WO1999037705A1) has been introduced in metal oxide self-assembly systems, uses segmented copolymer as structure directing agent, the carbon membrane of synthesizing ordered pore texture, charcoal fiber and charcoal piece.This method needs material cost higher, and the anti-inactivation stability of metal environment is low, circumstance complication, and reaction conditions is wayward.
Korean Patent (KR20120011460A) has been introduced a kind of take silicon as presoma, polymerization initiator, and tensio-active agent, transition metal mixes, a kind of crystallization Carbon Materials with order mesoporous structure of preparing by the heat treatment process of rare gas element.This method complicated operation, high expensive, environmental pollution load is larger.
Publication number be CN101367514 Introduction To Cn Patent one belong to technical field of inorganic nanometer material, relate to the method that organic formwork is prepared ordered mesoporous carbon.Take segmented copolymer as structure directing agent, resin is carbon precursor, and solid alkali is catalyzer, the organic/organic double compound carbon membrane that adopts sol-gel technique to be first self-assembled in non-aqueous solvent, and then charing obtains ordered mesoporous carbon.The present invention adopts segmented copolymer to assemble in alkaline non-aqueous solvent with resin to obtain, and organic/organic double compound has than the three-dimensional crosslinked network structure of high stable more of the synthetic product in acid system, directly char volume shrinks and subsides littlely, is easier to obtain ordered mesoporous carbon.The ordered mesoporous carbon that this method is prepared with simple method, but raw materials cost is high, and environmental protection not, awaits developing biomass material.
The Introduction To Cn Patent of publication number CN102977397A under a kind of room temperature, in ethanol-water solution, utilize the preparation method of the synthetic highly ordered mesosize pores resorcinol-formaldehyde polymer of resorcinol-formaldehyde resin and nonionogenic tenside and ordered mesoporous carbon.Concrete preparation process is, under basic catalyst, make the resorcinol-formaldehyde polymer precursor of low polymerization degree, by after polymer precursor and nonionic surfactant solution mixing, add an acidic catalyst, make the further polymerization around tensio-active agent of polymer precursor, and from solution Precipitation, centrifugal or the standing mixture that obtains polymer precursor-tensio-active agent after upper solution of removing, after mixture is dry in baking oven, under inert atmosphere, tensio-active agent is removed in roasting, obtain highly ordered mesosize pores macromolecular material, further at high temperature charing obtains corresponding ordered mesoporous carbon material.This preparation method's precipitation process is at room temperature carried out, consuming time short, acid base catalysator consumption is few, and the degree of order of the sharp material obtaining is in this way high, reproducible, and the process of formation polymer precursor-tensio-active agent is conducive in enormous quantities synthetic in liquid phase.But this method operating procedure complexity, high expensive, and environmental protection not, await developing a kind of biomass as raw material.
Publication number be CN102328924A Introduction To Cn Patent a kind of plant shell that utilizes manufacture the method for carbon molecular sieve, plant shell is ground into pulverulent material, to its be dried, abrasive dust is processed into micro-pulverulent material, then put into kneader with tackiness agent and carry out moulding, after moulding, material is put into converter and is carried out charing processing, obtains carbonaceous molecular sieve finished product by deposition of carbon.This method can effectively solve carbonaceous molecular sieve technique environmental pollution problem, is conducive to environment protection, but this method does not obtain orderly pore texture, limits its further application in adsorbing domain.
Publication number be CN101935032 Introduction To Cn Patent a kind of preparation method and its usage of molecular sieve, this method is with coal, coconut husk or resol etc. are raw material, after the conventional production stages such as pulverizing, moulding charing, steam activation, the shrinkage cavity of hydro carbons deposition, obtain a kind of carbon molecular sieve of routine, adopt re-activation technology to carry out reaming to conventional carbon molecular sieve, by regulation and control, it is carried out to modification.But this method also needs re-activation, operation steps complexity, increase time and reaction cost, and also pattern is uncontrollable.
Publication number be CN1899959 Introduction To Cn Patent a kind of preparation method of ordered mesoporous carbon material, the method is by Pluronic F-127-poly-propylene oxide-Pluronic F-127 triblock copolymer and sugary carbohydrates 4:1～3:1 in mass ratio, at 35 ℃, add in acid solution, through stirring, after dissolving, add again silicon source, the amount ratio of silicon source and sugary carbohydrates is 7～10ml/g, continue to stir 24h, by the solution obtaining crystallization 24～72h at 80～130 ℃ in airtight still, again through filtering, washing the at room temperature dry sugary carbohydrates that obtains, the ternary complex of triblock copolymer and silicon, by the pre-charing of ternary complex process, charing and silica removal finally obtain ordered mesoporous carbon.Ordered mesoporous carbon prepared by present method has that cheapness, carbon forming rate are high, the equal first-class feature of pore size distribution, it is raw material that this method has adopted biomass material sugary carbohydrates, the advantage that to have advocated biomass be raw material, select soft template method to prepare orderly Carbon Materials, but introduce silicon source, increase use cost, reactions steps complexity, production cycle is long, has increased reaction cost.
In sum, at present due to oil, Sweet natural gas day by day in short supply, biomass material is received extensive concern, simultaneously the raising to ordered mesoporous carbon real world applications performance requriements, control performance to mesoporous carbon pore structure also receives much concern, it is raw material that the present invention selects a kind of biomass, makes macromole become small molecules through the method for liquefaction, and pore structure is more easily controlled, soft template method through a kind of gentleness is structure directing agent, prepares the mesoporous carbon material of orderly pore texture after high-temperature calcination.
Summary of the invention:
The object of the present invention is to provide a kind of preparation method of soft template method tamarack base ordered mesoporous carbon.
In order to achieve the above object; the technical solution used in the present invention comprises: a kind of preparation method of soft template method tamarack base ordered mesoporous carbon; it is characterized in that: take larch sawdust as raw material; take phenol as liquefying agent; under acidic conditions; tamarack liquefaction is obtained to tamarack liquefied substance; react under alkaline condition with formaldehyde and generate resol; selecting segmented copolymer F127 is soft template; under acidic conditions, reaction generates the middle phase of tamarack base ordered mesoporous carbon; under nitrogen protection condition, obtain product through high-temperature calcination.The principal feature of this operating procedure is using biomass tamarack as raw material, abundant raw material, and resource reutilization, energy-saving and cost-reducing; By liquifying method, Litter Decomposition pine sill bits, more easily regulate and control its internal structure; Select gentle soft template segmented copolymer F127 to be successfully completed the regulation and control of ordered mesoporous carbon, pollute less, yield is high; Being convenient to industrial scale produces.
Advantage of the present invention is:
1, the utilization ratio that improves biomass energy take larch sawdust as raw material, raw materials cost is low, environmental protection.
2, the present invention has changed traditional production technique, uses liquefaction process, effectively controls the internal structure of timber.
3, select the internal structure of soft template method control Carbon Materials, save solvent load, reduce production costs, mesoporous carbon inverse amplification factor is higher, and yield is high.
4, high-temperature calcination under nitrogen protection, burn off soft template and impurity, form orderly pore texture, and this method sealing is pollution-free.
The present invention includes an accompanying drawing, accompanying drawing is described as follows: Fig. 1 is ordered mesoporous carbon structure iron
embodiment:
Below the invention process is described in further detail:
A kind of preparation method of soft template method tamarack base ordered mesoporous carbon; it is characterized in that: take larch sawdust as raw material; take phenol as liquefying agent; under acidic conditions, tamarack liquefaction is obtained to tamarack liquefied substance, react under alkaline condition with formaldehyde and generate resol; selecting segmented copolymer F127 is soft template; under acidic conditions, reaction generates the middle phase of tamarack base ordered mesoporous carbon, under nitrogen protection condition, obtains product through high-temperature calcination.The principal feature of this operating procedure is using biomass tamarack as raw material, abundant raw material, and resource reutilization, energy-saving and cost-reducing; By liquifying method, Litter Decomposition pine sill bits, more easily regulate and control its internal structure; Select gentle soft template segmented copolymer F127 to be successfully completed the regulation and control of ordered mesoporous carbon, pollute less, yield is high; Being convenient to industrial scale produces.
Below, the present invention will be further detailed with embodiment, but it is not limited to any or the similar example of these embodiment.
Embodiment 1:
Get 10g larch sawdust, 30g phenol, the 1mL vitriol oil (98%), 2mL phosphoric acid (85%) adds in there-necked flask, agitator and condenser post-heating are installed, and under reflux temperature, 110 ℃ of reaction 2h, stop heating, be cooled to after room temperature, add 80mL methyl alcohol, fully stir, mixed solution filters, after fully washing, collect filtrate.Filtrate is neutralized to neutrality with sodium hydroxide, filters insolubless such as removing salt, collect filtrate and remove methyl alcohol through underpressure distillation at 40 ℃, obtain brown liquefaction tamarack.
In flask, add successively 90mL formaldehyde solution (37%), 3g NaOH, add 10g F127, at 40 ℃, react 20h, add afterwards 10mL concentrated hydrochloric acid, regulating pH is 0.5, continue reaction 8h, after reaction finishes, be cooled to room temperature, through washing, baking oven inner drying at 100 ℃, obtains the middle phase of tamarack base mesoporous carbon.Molecular sieve carbon film preparation: by putting into mutually retort furnace in the middle of above-mentioned Molecular sieve carbon membranes, be warming up under 700 ℃ of carbonization temperatures, charing 2h, is cooled to room temperature and takes out, and obtains ordered mesoporous carbon.
Embodiment 2:
Get 10g larch sawdust, 30g phenol, the 2mL vitriol oil (98%), 2mL phosphoric acid (85%) adds in there-necked flask, agitator and condenser post-heating are installed, and under reflux temperature, 120 ℃ of reaction 2h, stop heating, be cooled to after room temperature, add 100mL methyl alcohol, fully stir, mixed solution filters, after fully washing, collect filtrate.Filtrate is neutralized to neutrality with sodium hydroxide, filters insolubless such as removing salt, collect filtrate and remove methyl alcohol through underpressure distillation at 40 ℃, obtain brown liquefaction tamarack.
In flask, add successively 80mL formaldehyde solution (37%), 3g NaOH, add 10g F127, at 40 ℃, react 18h, add afterwards 10mL concentrated hydrochloric acid, regulating pH is 0.5, continue reaction 10h, after reaction finishes, be cooled to room temperature, through washing, baking oven inner drying at 100 ℃, obtains the middle phase of tamarack base mesoporous carbon.Molecular sieve carbon film preparation: by putting into mutually retort furnace in the middle of above-mentioned Molecular sieve carbon membranes, be warming up under 700 ℃ of carbonization temperatures, charing 3h, is cooled to room temperature and takes out, and obtains ordered mesoporous carbon, sees accompanying drawing 1.
Claims (7)
1. the preparation method of a soft template method tamarack base ordered mesoporous carbon; it is characterized in that: take larch sawdust as raw material; take phenol as liquefying agent; under acidic conditions, tamarack liquefaction is obtained to tamarack liquefied substance, react under alkaline condition with formaldehyde and generate resol; selecting segmented copolymer F127 is soft template; under acidic conditions, reaction generates the middle phase of tamarack base ordered mesoporous carbon, under nitrogen protection condition, obtains product through high-temperature calcination.
2. according to the preparation method of a kind of soft template method tamarack base ordered mesoporous carbon claimed in claim 1, it is characterized in that: selecting these biomass of larch sawdust is raw material, raw material low cost, renewable, raw material abundance is secure, can replace part oil, the industrial chemicals such as coal simultaneously, reduce environmental pollution, improve the ecological environment.
3. according to the preparation method of a kind of soft template method tamarack base ordered mesoporous carbon claimed in claim 1, it is characterized in that: use the method for liquefaction, decompose wood internal structure, make its internal void structure more easily controlled.
4. according to the preparation method of a kind of soft template method tamarack base ordered mesoporous carbon claimed in claim 1, it is characterized in that: Liquefied wood is using under the acidic conditions of sulfuric acid and phosphate mixture, sulfuric acid and phosphate mixture total amount are 3～5mL, under alkaline condition, be prepared into thermosetting resin, amount of sodium hydroxide is 3～5g.
5. according to the preparation method of a kind of soft template method tamarack base ordered mesoporous carbon claimed in claim 1, it is characterized in that: selecting segmented copolymer is soft template, gentle controlled, pollution-free after removing, tensio-active agent shared 4%～7%, tensio-active agent, under strong acid condition, makes full use of and utilizes hydrogen bond action regulation and control pore texture, and pH is 3.
6. according to the preparation method of a kind of soft template method tamarack base ordered mesoporous carbon claimed in claim 1, it is characterized in that: 30～50 ℃ of temperature of reaction, reaction times 20～24h.
7. according to the preparation method of a kind of soft template method tamarack base ordered mesoporous carbon claimed in claim 1, it is characterized in that: calcining temperature is 700 ℃, calcination time 1～4h.
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Cited By (11)
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| CN104307383A (en) * | 2014-11-04 | 2015-01-28 | 东北林业大学 | Preparation method of larch-based ordered spherical porous structure carbon film |
| CN104386692A (en) * | 2014-11-04 | 2015-03-04 | 东北林业大学 | Preparation method of larch-based micro-mesoporous two-order porous carbon spheres |
| CN104386667A (en) * | 2014-11-04 | 2015-03-04 | 东北林业大学 | Method for preparing dahurian larch-based resin carbon aerogel microspheres |
| CN104445138A (en) * | 2014-11-04 | 2015-03-25 | 东北林业大学 | Method for preparing high-conductivity carbon material by virtue of hydrothermal method |
| CN106241770A (en) * | 2016-05-26 | 2016-12-21 | 浙江科技学院 | A kind of preparation method of bamboo base porous carbon |
| CN107335341A (en) * | 2017-04-26 | 2017-11-10 | 浙江大学 | A kind of preparation method of biological carbon membrane |
| CN108249418A (en) * | 2018-01-16 | 2018-07-06 | 南京农业大学 | A kind of high-specific surface area red bayberry core base graphene/ordered mesoporous carbon composite material and preparation method thereof |
| CN109019553A (en) * | 2018-07-18 | 2018-12-18 | 江苏科技大学 | It is a kind of with hard template method by the method and its application of cassia tree leaf synthesising biological matter carbon material |
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| CN109609151A (en) * | 2018-11-28 | 2019-04-12 | 大连理工大学 | Solid waste biomass prepares ordered mesopore carbon-metallic composite co-producing bio charcoal apparatus and method |
| CN113353917A (en) * | 2021-07-02 | 2021-09-07 | 哈尔滨师范大学 | Controllable preparation method of self-supporting two-dimensional mesoporous nano material |
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Cited By (17)
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| CN104386692A (en) * | 2014-11-04 | 2015-03-04 | 东北林业大学 | Preparation method of larch-based micro-mesoporous two-order porous carbon spheres |
| CN104386667A (en) * | 2014-11-04 | 2015-03-04 | 东北林业大学 | Method for preparing dahurian larch-based resin carbon aerogel microspheres |
| CN104445138A (en) * | 2014-11-04 | 2015-03-25 | 东北林业大学 | Method for preparing high-conductivity carbon material by virtue of hydrothermal method |
| CN104445138B (en) * | 2014-11-04 | 2016-08-24 | 东北林业大学 | A kind of hydro-thermal method prepares the method for high conductivity Carbon Materials |
| CN104307383A (en) * | 2014-11-04 | 2015-01-28 | 东北林业大学 | Preparation method of larch-based ordered spherical porous structure carbon film |
| CN106241770B (en) * | 2016-05-26 | 2019-03-08 | 浙江科技学院 | A kind of preparation method of bamboo base porous carbon |
| CN106241770A (en) * | 2016-05-26 | 2016-12-21 | 浙江科技学院 | A kind of preparation method of bamboo base porous carbon |
| CN107335341B (en) * | 2017-04-26 | 2019-12-17 | 浙江大学 | Preparation method of biological carbon film |
| CN107335341A (en) * | 2017-04-26 | 2017-11-10 | 浙江大学 | A kind of preparation method of biological carbon membrane |
| CN108249418A (en) * | 2018-01-16 | 2018-07-06 | 南京农业大学 | A kind of high-specific surface area red bayberry core base graphene/ordered mesoporous carbon composite material and preparation method thereof |
| CN108249418B (en) * | 2018-01-16 | 2023-07-21 | 南京农业大学 | High specific surface area myrica rubra nuclear-based graphene/ordered mesoporous carbon composite material and preparation method thereof |
| CN109019553A (en) * | 2018-07-18 | 2018-12-18 | 江苏科技大学 | It is a kind of with hard template method by the method and its application of cassia tree leaf synthesising biological matter carbon material |
| CN109395703A (en) * | 2018-07-31 | 2019-03-01 | 中山大学 | A kind of poly-dopamine molecular engram ordered mesoporous carbon material and preparation method thereof |
| CN109395703B (en) * | 2018-07-31 | 2021-08-31 | 中山大学 | Polydopamine molecularly imprinted ordered mesoporous carbon material and preparation method thereof |
| CN109609151A (en) * | 2018-11-28 | 2019-04-12 | 大连理工大学 | Solid waste biomass prepares ordered mesopore carbon-metallic composite co-producing bio charcoal apparatus and method |
| CN109609151B (en) * | 2018-11-28 | 2021-01-05 | 大连理工大学 | Device and method for preparing ordered mesoporous carbon-metal composite material from solid waste biomass |
| CN113353917A (en) * | 2021-07-02 | 2021-09-07 | 哈尔滨师范大学 | Controllable preparation method of self-supporting two-dimensional mesoporous nano material |
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Application publication date: 20140604 |