CN107628620A - A kind of method that nitrogen carbon molecular sieve is prepared by bagasse - Google Patents
A kind of method that nitrogen carbon molecular sieve is prepared by bagasse Download PDFInfo
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- CN107628620A CN107628620A CN201710903182.7A CN201710903182A CN107628620A CN 107628620 A CN107628620 A CN 107628620A CN 201710903182 A CN201710903182 A CN 201710903182A CN 107628620 A CN107628620 A CN 107628620A
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Abstract
The invention discloses a kind of method that nitrogen carbon molecular sieve is prepared by bagasse, the raw material of use are bagasse, its wide material sources, and cheap；The carbon molecular sieve uniform pore diameter of preparation, it is adapted to nitrogen to prepare, is a kind of new Application way 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 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 a kind of prepares nitrogen carbon molecular sieve by bagasse
Method.
A kind of method that 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：Solution is handled into 30-40min in the case where frequency is 25-35KHz ultrasonic wave, filters, collects 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.
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, it is adapted to nitrogen to prepare, is a kind of the new of bagasse
Application way.
Embodiment
Embodiment 1：
A kind of method that 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：Solution is handled into 35min in the case where frequency is 28KHz ultrasonic wave, filters, collects 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.
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 bagasse weight
0.04%, 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 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：Solution is handled into 40min in the case where frequency is 35KHz ultrasonic wave, filters, collects 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.
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 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：Solution is handled into 40min in the case where frequency is 25KHz ultrasonic wave, filters, collects 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.
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
Carburizing temperature in embodiment 1 is adjusted, other preparation conditions are constant, and final molecular sieve compares surface after being carbonized
Long-pending relation is as follows：
By above test data it is recognised that the carburizing temperature of raw material has a great influence to molecular sieve specific surface area, carburizing temperature
More than 950 DEG C, the size variation of specific surface area is little, and preferable carburizing temperature of the invention is 950-1000 DEG C.
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 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 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：Solution is handled into 35min in the case where frequency is 28KHz ultrasonic wave, filters, collects 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,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.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710903182.7A CN107628620A (en) | 2016-07-09 | 2016-07-09 | A kind of method that nitrogen carbon molecular sieve is prepared by bagasse |
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| CN201710903182.7A CN107628620A (en) | 2016-07-09 | 2016-07-09 | A kind of method that nitrogen carbon molecular sieve is prepared by bagasse |
| CN201610536806.1A CN106185915B (en) | 2016-07-09 | 2016-07-09 | A kind of method that nitrogen carbon molecular sieve is prepared by bagasse |
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| CN201710903185.0A Withdrawn CN107529517A (en) | 2016-07-09 | 2016-07-09 | A kind of method that nitrogen carbon molecular sieve is prepared by bagasse |
| CN201710903182.7A Withdrawn CN107628620A (en) | 2016-07-09 | 2016-07-09 | A kind of method that nitrogen carbon molecular sieve is prepared by bagasse |
| CN201710903183.1A Withdrawn CN107529515A (en) | 2016-07-09 | 2016-07-09 | A kind of method that nitrogen carbon molecular sieve is prepared by bagasse |
| CN201610536806.1A Active CN106185915B (en) | 2016-07-09 | 2016-07-09 | A kind of method that nitrogen carbon molecular sieve is prepared by bagasse |
| CN201710903181.2A Withdrawn CN107572521A (en) | 2016-07-09 | 2016-07-09 | A kind of method that nitrogen carbon molecular sieve is prepared by bagasse |
| CN201710903085.8A Withdrawn CN107572520A (en) | 2016-07-09 | 2016-07-09 | A kind of method that nitrogen carbon molecular sieve is prepared by bagasse |
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| CN201610536806.1A Active CN106185915B (en) | 2016-07-09 | 2016-07-09 | A kind of method that nitrogen carbon molecular sieve is prepared by bagasse |
| CN201710903181.2A Withdrawn CN107572521A (en) | 2016-07-09 | 2016-07-09 | A kind of method that nitrogen carbon molecular sieve is prepared by bagasse |
| CN201710903085.8A Withdrawn CN107572520A (en) | 2016-07-09 | 2016-07-09 | A kind of method that nitrogen carbon molecular sieve is prepared by bagasse |
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| CN109453745A (en) * | 2018-12-28 | 2019-03-12 | 苏州班顺工业气体设备有限公司 | High strength carbon molecular sieve and preparation method thereof |
Citations (1)
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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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| Publication number | Priority date | Publication date | Assignee | Title |
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| ZA815721B (en) * | 1980-08-26 | 1983-01-26 | Boyd Terence Keogh | Bagasse residue filter materials and activated carbon products and methods of manufacturing same |
| 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 |
| CN101696006B (en) * | 2009-05-21 | 2011-08-03 | 安徽建筑工业学院 | Method for preparing carbon molecular sieve |
| CN102206691B (en) * | 2011-03-26 | 2012-05-23 | 北海田野食品有限公司 | Method for producing xylose oligomer from bagasse |
| CN102964393B (en) * | 2012-11-30 | 2014-12-03 | 安徽丰原发酵技术工程研究有限公司 | Method for producing xylose by use of xylose mother liquid |
| CN103241737B (en) * | 2013-05-29 | 2015-07-01 | 广西大学 | Sludge bagasse active carbon and preparation method thereof |
| CN103333265B (en) * | 2013-06-05 | 2016-03-30 | 南方医科大学 | A kind of method of bagasse separation of polysaccharides purifying |
| CN103349973B (en) * | 2013-06-14 | 2015-05-06 | 湖州新奥利吸附材料有限公司 | Regeneration method of nitrogen-preparation carbon molecular sieve |
| 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 |
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2016
- 2016-07-09 CN CN201710903184.6A patent/CN107529516A/en not_active Withdrawn
- 2016-07-09 CN CN201710903185.0A patent/CN107529517A/en not_active Withdrawn
- 2016-07-09 CN CN201710903182.7A patent/CN107628620A/en not_active Withdrawn
- 2016-07-09 CN CN201710903183.1A patent/CN107529515A/en not_active Withdrawn
- 2016-07-09 CN CN201610536806.1A patent/CN106185915B/en active Active
- 2016-07-09 CN CN201710903181.2A patent/CN107572521A/en not_active Withdrawn
- 2016-07-09 CN CN201710903085.8A patent/CN107572520A/en not_active Withdrawn
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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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Also Published As
| Publication number | Publication date |
|---|---|
| CN107572521A (en) | 2018-01-12 |
| CN107529515A (en) | 2018-01-02 |
| CN106185915A (en) | 2016-12-07 |
| CN107529517A (en) | 2018-01-02 |
| CN107529516A (en) | 2018-01-02 |
| CN106185915B (en) | 2017-12-22 |
| CN107572520A (en) | 2018-01-12 |
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Application publication date: 20180126 |