CN107572516A - A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse - Google Patents
A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse Download PDFInfo
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- CN107572516A CN107572516A CN201710903083.9A CN201710903083A CN107572516A CN 107572516 A CN107572516 A CN 107572516A CN 201710903083 A CN201710903083 A CN 201710903083A CN 107572516 A CN107572516 A CN 107572516A
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- bagasse
- molecular sieve
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- nitrogen
- surface area
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P1/00—Preparation of compounds or compositions, not provided for in groups C12P3/00 - C12P39/00, by using microorganisms or enzymes
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P2201/00—Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
Abstract
The invention discloses a kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse, the raw material of use are bagasse, its wide material sources, and cheap；Carbon molecular sieve uniform pore diameter, the specific surface area of preparation are high, by adjustment aperture, are adapted to nitrogen to prepare, and are a kind of new Application ways of bagasse.
Description
Technical field
The present invention relates to a kind of preparation method of molecular sieve, belongs to carbon materials field, more particularly to one kind by bagasse
The method for preparing high-specific surface area nitrogen carbon molecular sieve.
Background technology
Carbon molecular sieve is a kind of carbonaceous porous material, belongs to one kind of activated carbon.Its cavity is mainly by below 1nm micropore
Formed with a small amount of macropore, pore-size distribution is narrower, about in 0.5-1.0nm or so.And normal activated carbon also has big in addition to micropore
The mesopore and macropore of amount, average pore size is in 2nm or so.The hole of carbon molecular sieve is slit-type.Available for the original for preparing carbon molecular sieve
Material is very extensive, may serve to manufacture carbon molecular sieve from natural products to high molecular polymer.Wherein most important three kinds are
Coal, timber, shell, the report for using bagasse to prepare carbon molecular sieve for raw material is not seen.
Shanghai Communications University discloses one kind in Chinese invention patent CN1472134A and prepares carbon molecular sieve by pomace
Method, but this method prepare carbon molecular sieve aperture be 6.2-10 angstroms, the size in aperture and the scope in aperture are much larger than
The requirement of nitrogen molecule sieve.
Sugarcane is one of primary raw material of sugaring.The remaining bagasse after squeezing sugar, there are about 50% fiber can use
Carry out papermaking.But, wherein still there is part sugarcane marrow（Myelocyte）Do not interweave power, should be removed before pulping process.Bagasse fibre
Length is about 0.65-2.17mm, and width is 21-28 μm.Although its fibre morphology is less than timber and bamboo, than rice,
Wheat straw fiber is then slightly better.After slurry can be incorporated part wood pulp, offset printing paper processed, cement bag paper etc. are copied.
The content of the invention
Based on technical problem existing for background technology, the present invention proposes one kind and prepares high-specific surface area nitrogen by bagasse
The method of carbon molecular sieve.
A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse, comprises the following steps：
Step 1：Bagasse is carried out after simply cleaning, by its mechanical crushing to 1-3mm, by being steam heated to 190-
260 DEG C, 2-5min is maintained, then the abrupt release pressure within the 0.1-1s times, makes bagasse cell wall fiber expanded, obtain swollen
It is standby to change bagasse；
Step 2：The enzyme solutions that expanded bagasse is soaked in 10-15 times of volume hydrolyze 15- at pH4-5,90-100 DEG C
25min；
Step 3：Micro fullerene is added in the solution, and solution is handled into 30- in the case where frequency is 25-35KHz ultrasonic wave
40min, filtering, collect filtrate；
Step 4：Adding ethanol makes its concentration in filtrate be settled out bagasse polysaccharide solid, and vacuum is done to 80-90%
It is dry, obtain bagasse polysaccharide solid；
Step 5：Bagasse polysaccharide solid is put into carbide furnace, raw material are laid naturally in the plane, temperature is risen into charcoal
Change temperature, charing obtains carbon molecular sieve；
Step 6：Carbon molecular sieve is placed in converter, 950-1000 DEG C is warming up under nitrogen guard mode, shape is protected in nitrogen
Benzene is passed through under state aperture adjustment is carried out to carbon molecular sieve, obtain nitrogen carbon molecular sieve.
Preferably, described fullerene is football alkene C60, and addition is the 0.03-0.08% of bagasse weight.
C60 is a kind of Spectra of Carbon Clusters, is marked by 14C.It is made up of the 32 face bodies as football 60 carbon atoms, including
20 hexagons, 12 pentagons.When this 60 C atoms are arranged in space, a most stable of space of chemical bond is formed
Arrangement position, it is just consistent with the arrangement of football surface lattice.Because the proposition of this structure is by building scholar's fowler
(Buckminster Fuller）Inspiration.Fowler once designed a kind of thin spherical shell formed with hexagon and pentagon and builds knot
Structure.Therefore C60 is called football alkene, also referred to as fullerene (Fullerence) by scientist.
The diameter of C60 molecules is about 7.1 angstroms, micro to be added in polysaccharide solid, can make polysaccharide molecule using it as template,
It is more preferably scattered to obtain particle diameter, the higher carbon molecular sieve of specific surface area.
Preferably, described enzyme includes cellulase, papain and pectase.
Preferably, the gross weight of described enzyme is the 0.05-0.2% of bagasse weight.
Preferably, described carburizing temperature is 950-1000 DEG C.
Be carbonized pre-treatment, it is necessary to through over cleaning, swelling of fiber, enzyme decomposition, supersound process to bagasse in the present invention
And dry, bagasse is really converted into the uniform polysaccharide solid of particle size by these steps, then again by polysaccharide
The optimum choice of thickness and carburizing temperature when the particle diameter of solid and carbonization, finally give and meet nitrogen carbon molecular sieve requirement
Preparation method.
Chinese invention patent CN101171956 discloses a kind of method that polysaccharide is extracted from bagasse, and this method passes through
Degreasing, ferment treatment, ultrasonic extraction and alcohol precipitation obtain bagasse polysaccharide solid.The present invention in contrast, in opening for sugarcane Slag treatment
It is expanded that stage beginning first carries out cell wall fiber, has the following advantages that：First, to the enzyme needed for follow-up ferment treatment and ultrasonic extraction
Time needed for reason, the condition such as the concentration of enzyme and the frequency of ultrasonic extraction and time have all lowered, and save raw material and energy
Source；Second, after cell wall fiber is expanded, the particle diameter of manufactured bagasse polysaccharide solid will uniformly much, and this is to prepare nitrogen
Condition necessary to gas molecular sieve.
Because nitrogen（30 angstroms）And oxygen（28 angstroms）Particle diameter difference it is minimum, and nitrogen molecule sieve need oxygen and nitrogen
It is separated, therefore when preparing nitrogen molecule sieve, the uniform particle sizes of raw material, small pore diameter range is primary condition.
The present invention and the manufacture method of the carbon molecular sieve in background technology, the raw material that the present invention uses are bagasse, its
Wide material sources, and it is cheap；The carbon molecular sieve uniform pore diameter of preparation, specific surface area is high, after adjustment aperture, is adapted to nitrogen
Prepared by gas, be a kind of new Application way of bagasse.
Embodiment
Embodiment 1：
A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse, comprises the following steps：
Step 1：Bagasse is carried out after simply cleaning, by its mechanical crushing to 1-3mm, by being steam heated to 220 DEG C,
5min is maintained, then the abrupt release pressure within the 0.5s times, makes bagasse cell wall fiber expanded, it is standby to obtain expanded bagasse
With；
Step 2：The enzyme solutions that expanded bagasse is soaked in 12 times of volumes hydrolyze 20min at pH4-5,90-100 DEG C；
Step 3：Micro C60 is added in the solution, and solution is handled into 35min in the case where frequency is 28KHz ultrasonic wave, is filtered,
Collect filtrate；
Step 4：Adding ethanol makes its concentration in filtrate be settled out bagasse polysaccharide solid to 85%, and is dried in vacuo,
Obtain bagasse polysaccharide solid；
Step 5：Bagasse polysaccharide solid is put into carbide furnace, raw material are laid naturally in the plane, temperature is risen into charcoal
Change temperature, charing obtains carbon molecular sieve；
Step 6：Carbon molecular sieve is placed in converter, 950 DEG C are warming up under nitrogen guard mode, under nitrogen guard mode
It is passed through benzene and aperture adjustment is carried out to carbon molecular sieve, obtains nitrogen carbon molecular sieve；
Described C60 addition is the 0.05% of bagasse weight；
Described enzyme includes cellulase, papain and pectase；
The gross weight of described enzyme is the 0.1% of bagasse weight, and the weight of its cellulase is the 0.04% of bagasse weight,
Papain weight is the 0.04% of bagasse weight, and pectase weight is the 0.02% of bagasse weight；
Described carburizing temperature is 980 DEG C.
Embodiment 2：
A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse, comprises the following steps：
Step 1：Bagasse is carried out after simply cleaning, by its mechanical crushing to 1-3mm, by being steam heated to 260 DEG C,
2min is maintained, then the abrupt release pressure within the 0.1s times, makes bagasse cell wall fiber expanded, it is standby to obtain expanded bagasse
With；
Step 2：The enzyme solutions that expanded bagasse is soaked in 10 times of volumes hydrolyze 25min at pH4-5,90 DEG C；
Step 3：Micro C60 is added in the solution, and solution is handled into 40min in the case where frequency is 35KHz ultrasonic wave, is filtered,
Collect filtrate；
Step 4：Adding ethanol makes its concentration in filtrate be settled out bagasse polysaccharide solid to 90%, and is dried in vacuo,
Obtain bagasse polysaccharide solid；
Step 5：Bagasse polysaccharide solid is put into carbide furnace, raw material are laid naturally in the plane, temperature is risen into charcoal
Change temperature, charing obtains carbon molecular sieve；
Step 6：Carbon molecular sieve is placed in converter, 1000 DEG C are warming up under nitrogen guard mode, under nitrogen guard mode
It is passed through benzene and aperture adjustment is carried out to carbon molecular sieve, obtains nitrogen carbon molecular sieve.
Described C60 addition is the 0.03% of bagasse weight；
Described enzyme includes cellulase, papain and pectase.
The gross weight of described enzyme is the 0.2% of bagasse weight, and the weight of its cellulase is bagasse weight
0.05%, papain weight is the 0.1% of bagasse weight, and pectase weight is the 0.05% of bagasse weight.
Described carburizing temperature is 950 DEG C.
Embodiment 3：
A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse, comprises the following steps：
Step 1：Bagasse is carried out after simply cleaning, by its mechanical crushing to 1-3mm, by being steam heated to 190 DEG C,
5min is maintained, then the abrupt release pressure within the 1s times, makes bagasse cell wall fiber expanded, it is standby to obtain expanded bagasse
With；
Step 2：The enzyme solutions that expanded bagasse is soaked in 10 times of volumes hydrolyze 15min at pH4-5,90 DEG C；
Step 3：Micro C60 is added in the solution, and solution is handled into 40min in the case where frequency is 25KHz ultrasonic wave, is filtered,
Collect filtrate；
Step 4：Adding ethanol makes its concentration in filtrate be settled out bagasse polysaccharide solid to 80%, and is dried in vacuo,
Obtain bagasse polysaccharide solid；
Step 5：Bagasse polysaccharide solid is put into carbide furnace, raw material are laid naturally in the plane, temperature is risen into charcoal
Change temperature, charing obtains carbon molecular sieve.
Step 6：Carbon molecular sieve is placed in converter, 970 DEG C are warming up under nitrogen guard mode, shape is protected in nitrogen
Benzene is passed through under state aperture adjustment is carried out to carbon molecular sieve, obtain nitrogen carbon molecular sieve.
Described C60 addition is the 0.08% of bagasse weight
Described enzyme includes cellulase, papain and pectase.
The gross weight of described enzyme is the 0.05% of bagasse weight, and the weight of its cellulase is bagasse weight
0.03%, papain weight is the 0.01% of bagasse weight, and pectase weight is the 0.01% of bagasse weight.
Described carburizing temperature is 1000 DEG C.
Comparative example 1
C60 in embodiment 1 is removed, other preparation conditions are constant, the survey of final molecular sieve specific surface area after being carbonized
It is as follows to try data：
By above test data it is recognised that influences of the addition C60 to the specific surface area of the molecular sieve of the present invention is very big.
It is only the preferable embodiment of the present invention described in above example, but protection scope of the present invention not office
Be limited to this, any one skilled in the art the invention discloses technical scope in, the technique according to the invention
Scheme and its inventive concept are subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (1)
- A kind of 1. method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse, it is characterised in that comprise the following steps：Step 1：Bagasse is carried out after simply cleaning, by its mechanical crushing to 1-3mm, by being steam heated to 190-260 DEG C, 2-5min is maintained, then the abrupt release pressure within the 0.1-1s times, makes bagasse cell wall fiber expanded, obtain expanded Bagasse is standby；Step 2：The enzyme solutions that expanded bagasse is soaked in 10-15 times of volume hydrolyze 15- at pH4-5,90-100 DEG C 25min；Step 3：Micro fullerene is added in the solution, and solution is handled into 30- in the case where frequency is 25-35KHz ultrasonic wave 40min, filtering, collect filtrate；Step 4：Adding ethanol makes its concentration in filtrate be settled out bagasse polysaccharide solid, and vacuum is done to 80-90% It is dry, obtain bagasse polysaccharide solid；Step 5：Bagasse polysaccharide solid is put into carbide furnace, raw material are laid naturally in the plane, temperature is risen into charcoal Change temperature, charing obtains carbon molecular sieve；Step 6：Carbon molecular sieve is placed in converter, 950-1000 DEG C is warming up under nitrogen guard mode, shape is protected in nitrogen Benzene is passed through under state aperture adjustment is carried out to carbon molecular sieve, obtain nitrogen carbon molecular sieve;Described carburizing temperature is 950-1000 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710903083.9A CN107572516A (en) | 2016-07-09 | 2016-07-09 | A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse |
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| CN201710903083.9A CN107572516A (en) | 2016-07-09 | 2016-07-09 | A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse |
| CN201610537404.3A CN106185916B (en) | 2016-07-09 | 2016-07-09 | A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse |
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| CN201710903171.9A Expired - Fee Related CN107555432B (en) | 2016-07-09 | 2016-07-09 | Method for preparing nitrogen carbon molecular sieve with high specific surface area from bagasse |
| CN201710903172.3A Withdrawn CN107777684A (en) | 2016-07-09 | 2016-07-09 | A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse |
| CN201710903174.2A Withdrawn CN107673349A (en) | 2016-07-09 | 2016-07-09 | A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse |
| CN201710903083.9A Withdrawn CN107572516A (en) | 2016-07-09 | 2016-07-09 | A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse |
| CN201710903089.6A Withdrawn CN107792852A (en) | 2016-07-09 | 2016-07-09 | A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse |
| CN201710903175.7A Withdrawn CN107619048A (en) | 2016-07-09 | 2016-07-09 | A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse |
| CN201610537404.3A Active CN106185916B (en) | 2016-07-09 | 2016-07-09 | A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse |
| CN201710903084.3A Withdrawn CN107585766A (en) | 2016-07-09 | 2016-07-09 | A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse |
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| CN201710903171.9A Expired - Fee Related CN107555432B (en) | 2016-07-09 | 2016-07-09 | Method for preparing nitrogen carbon molecular sieve with high specific surface area from bagasse |
| CN201710903172.3A Withdrawn CN107777684A (en) | 2016-07-09 | 2016-07-09 | A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse |
| CN201710903174.2A Withdrawn CN107673349A (en) | 2016-07-09 | 2016-07-09 | A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse |
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| CN201710903175.7A Withdrawn CN107619048A (en) | 2016-07-09 | 2016-07-09 | A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse |
| CN201610537404.3A Active CN106185916B (en) | 2016-07-09 | 2016-07-09 | A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse |
| CN201710903084.3A Withdrawn CN107585766A (en) | 2016-07-09 | 2016-07-09 | A kind of method that high-specific surface area nitrogen carbon molecular sieve is prepared by bagasse |
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| CN107974093A (en) * | 2017-12-21 | 2018-05-01 | 许炜玮 | A kind of road and bridge filleting pitch and preparation method thereof |
| CN109369070A (en) * | 2018-11-20 | 2019-02-22 | 黎剑华 | A kind of asphalt pavement material and preparation method thereof that acid rain resistant corrodes |
| CN111150695A (en) * | 2020-01-14 | 2020-05-15 | 浙江神英科技股份有限公司 | Preparation method of hand sanitizer with super-strong decontamination effect |
| CN111303658A (en) * | 2020-03-16 | 2020-06-19 | 齐齐哈尔大学 | Environment-friendly pigment free of heavy metal and preparation method thereof |
| WO2021212406A1 (en) * | 2020-04-23 | 2021-10-28 | 浙江华彩新材料有限公司 | Haa low temperature curing super-leveling weatherable powder coating |
| CN111924839A (en) * | 2020-08-18 | 2020-11-13 | 湖州民强炭业有限公司 | Preparation method of nitrogen-making carbon molecular sieve by taking gordon euryale seed shell as raw material |
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| CN103435819A (en) * | 2013-07-17 | 2013-12-11 | 青岛科技大学 | Method for preparing thread-shaped polyaniline micro-nano tubes with fullerene fiber as template and products of thread-shaped polyaniline micro-nano tubes |
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| CN1202992C (en) * | 2003-06-05 | 2005-05-25 | 上海交通大学 | Method for preparing carbon molecular sieve from apple dregs |
| CN101171956B (en) * | 2007-11-27 | 2010-07-21 | 南方医科大学 | Method for extracting polyoses from bagasse |
| CN104722134B (en) * | 2013-12-24 | 2016-08-31 | 张逸 | A kind of centrifuge equipment for separating liquid from solid |
| CN103803547B (en) * | 2014-02-17 | 2015-12-02 | 江苏竹海活性炭有限公司 | A kind of method utilizing bagasse to prepare foodstuff sanitation-stage gac |
| CN105152156B (en) * | 2015-08-14 | 2017-04-12 | 湖州新奥利吸附材料有限公司 | Preparation technology of high-performance carbon molecular sieve |
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2016
- 2016-07-09 CN CN201710903171.9A patent/CN107555432B/en not_active Expired - Fee Related
- 2016-07-09 CN CN201710903172.3A patent/CN107777684A/en not_active Withdrawn
- 2016-07-09 CN CN201710903174.2A patent/CN107673349A/en not_active Withdrawn
- 2016-07-09 CN CN201710903083.9A patent/CN107572516A/en not_active Withdrawn
- 2016-07-09 CN CN201710903089.6A patent/CN107792852A/en not_active Withdrawn
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- 2016-07-09 CN CN201610537404.3A patent/CN106185916B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435819A (en) * | 2013-07-17 | 2013-12-11 | 青岛科技大学 | Method for preparing thread-shaped polyaniline micro-nano tubes with fullerene fiber as template and products of thread-shaped polyaniline micro-nano tubes |
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| 刘佳等: "碳分子筛制备技术研究进展及应用", 《化工生产与技术》 * |
| 郦金龙等: "酶水解制备玉米芯喷爆渣可溶性膳食纤维", 《中国食品学报》 * |
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| Publication number | Publication date |
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| CN107555432B (en) | 2020-06-19 |
| CN107555432A (en) | 2018-01-09 |
| CN106185916B (en) | 2017-12-26 |
| CN107777684A (en) | 2018-03-09 |
| CN107792852A (en) | 2018-03-13 |
| CN107673349A (en) | 2018-02-09 |
| CN106185916A (en) | 2016-12-07 |
| CN107585766A (en) | 2018-01-16 |
| CN107619048A (en) | 2018-01-23 |
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Application publication date: 20180112 |