CN107555432B - Method for preparing nitrogen carbon molecular sieve with high specific surface area from bagasse - Google Patents
Method for preparing nitrogen carbon molecular sieve with high specific surface area from bagasse Download PDFInfo
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- CN107555432B CN107555432B CN201710903171.9A CN201710903171A CN107555432B CN 107555432 B CN107555432 B CN 107555432B CN 201710903171 A CN201710903171 A CN 201710903171A CN 107555432 B CN107555432 B CN 107555432B
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- bagasse
- molecular sieve
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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
- 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
- C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
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- C—CHEMISTRY; METALLURGY
- 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 method for preparing a nitrogen carbon molecular sieve with high specific surface area from bagasse, which adopts the bagasse as a raw material, and has wide source and low price; the prepared carbon molecular sieve has uniform aperture and high specific surface area, is suitable for nitrogen preparation by adjusting the aperture, and is a novel utilization method of bagasse.
Description
Technical Field
The invention relates to a preparation method of a molecular sieve, belongs to the field of carbon materials, and particularly relates to a method for preparing a nitrogen carbon molecular sieve with a high specific surface area from bagasse.
Background
The carbon molecular sieve is a carbon porous material, and belongs to one type of activated carbon. The cavity is mainly composed of micropores with the diameter of less than 1nm and a small amount of macropores, and the pore size distribution is narrow and is about 0.5-1.0 nm. The common active carbon has a large amount of mesopores and macropores besides micropores, and the average pore diameter is about 2 nm. The pores of the carbon molecular sieve are slit type. The raw materials which can be used for preparing the carbon molecular sieve are very wide, and the carbon molecular sieve can be prepared from natural products to high molecular polymers. The most main three of the raw materials are coal, wood and fruit shells, and reports of preparing the carbon molecular sieve by using bagasse as a raw material are not seen.
The Shanghai university of transportation in Chinese patent CN1472134A discloses a method for preparing a carbon molecular sieve from apple pomace, but the pore diameter of the carbon molecular sieve prepared by the method is 6.2-10 angstroms, and the pore size and the pore diameter range are far larger than the requirements of a nitrogen molecular sieve.
Sugarcane is one of the main raw materials for sugar production. About 50% of the fiber of the bagasse, which remains after sugar pressing, can be used for paper making. However, some of the pith (marrow cells) have no interweaving force and should be removed before pulping. The bagasse fibers are about 0.65-2.17 mm in length and 21-28 μm in width. Although the fiber form is inferior to wood and bamboo, the fiber form is better than rice and wheat straw fiber. The pulp can be mixed with part of wood pulp to make offset printing paper, cement bag paper, etc.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a method for preparing a nitrogen carbon molecular sieve with high specific surface area from bagasse.
A method for preparing a nitrogen carbon molecular sieve with high specific surface area from bagasse comprises the following steps:
the method comprises the following steps: simply cleaning bagasse, mechanically crushing the bagasse to 1-3mm, heating the bagasse to 260 ℃ by steam, maintaining the temperature for 2-5min, and then instantly releasing pressure within 0.1-1s to expand bagasse cell wall fibers to obtain expanded bagasse for later use;
step two: soaking puffed bagasse in 10-15 times volume of enzyme solution, hydrolyzing at 90-100 deg.C and pH of 4-5 for 15-25 min;
step three: adding micro fullerene into the solution, treating the solution for 30-40min under ultrasonic wave with frequency of 25-35KHz, filtering, and collecting filtrate;
step four: adding ethanol to make the concentration of the ethanol in the filtrate reach 80-90%, precipitating bagasse polysaccharide solid, and vacuum drying to obtain bagasse polysaccharide solid;
step five: putting the bagasse polysaccharide solid into a carbonization furnace, naturally laying the raw material on a plane, raising the temperature to a carbonization temperature, and carbonizing to obtain the carbon molecular sieve;
step six: and (3) placing the carbon molecular sieve in a converter, heating to 950-1000 ℃ under the protection of nitrogen, and introducing benzene to adjust the aperture of the carbon molecular sieve under the protection of nitrogen to obtain the nitrogen carbon molecular sieve.
Preferably, the fullerene is football C60, and the addition amount is 0.03-0.08% of the weight of the bagasse.
C60 is a carbon atom cluster, labeled 14C. It is composed of 60 carbon atoms, and is a 32-sided body like a football, comprising 20 hexagons and 12 pentagons. When the 60C atoms are arranged in space, a spatial arrangement position with the most stable chemical bonds is formed, and the arrangement position is just consistent with the arrangement of the lattices on the surface of the football. Since the proposal of this structure was inspired by architects' fullers (Buckminster Fuller). Fullerenes have designed a spherical shell building structure made of hexagons and pentagons. Scientists have thus called C60 football, also called fullerene (Fullerence).
The diameter of C60 molecule is about 7.1 angstrom, and when adding into polysaccharide solid in a small amount, it can make the polysaccharide molecule use it as template to obtain carbon molecular sieve with better dispersion of particle size and higher specific surface area.
Preferably, the enzymes include cellulase, papain and pectinase.
Preferably, the total weight of the enzyme is 0.05-0.2% of the weight of the bagasse.
Preferably, the carbonization temperature is 950-.
In the invention, bagasse is subjected to carbonization pretreatment, and is required to be subjected to cleaning, fiber puffing, enzyme decomposition, ultrasonic treatment and drying, the bagasse is actually converted into polysaccharide solid with uniform particle size, and then the particle size, the thickness during carbonization and the carbonization temperature of the polysaccharide solid are optimally selected, so that the preparation method meeting the requirements of the nitrogen-carbon molecular sieve is finally obtained.
Chinese patent CN101171956 discloses a method for extracting polysaccharide from bagasse, which comprises degreasing, enzyme treatment, ultrasonic extraction and alcohol precipitation to obtain bagasse polysaccharide solid. Compared with the method, the method firstly performs cell wall fiber expansion at the initial stage of bagasse treatment, and has the following advantages: firstly, the time required by enzyme treatment required by subsequent enzyme treatment and ultrasonic extraction, the concentration of the enzyme, the frequency and time of ultrasonic extraction and other conditions are reduced, and raw materials and energy are saved; secondly, after the cell wall fibers are expanded, the grain size of the prepared bagasse polysaccharide solid is much more uniform, which is the necessary condition for preparing the nitrogen molecular sieve.
Since the particle size difference between nitrogen (30 angstroms) and oxygen (28 angstroms) is very small, and the nitrogen molecular sieve needs to separate oxygen from nitrogen, the uniform particle size of the raw material and the small pore size range are the basic conditions in the preparation of the nitrogen molecular sieve.
Compared with the manufacturing method of the carbon molecular sieve in the background art, the raw material adopted by the invention is bagasse, which has wide source and low price; the prepared carbon molecular sieve has uniform aperture and high specific surface area, is suitable for nitrogen preparation after aperture adjustment, and is a novel utilization method of bagasse.
Detailed Description
Example 1:
a method for preparing a nitrogen carbon molecular sieve with high specific surface area from bagasse comprises the following steps:
the method comprises the following steps: simply cleaning bagasse, mechanically pulverizing to 1-3mm, heating to 220 deg.C with steam, maintaining for 5min, and instantaneously releasing pressure within 0.5s to swell cell wall fiber of bagasse to obtain puffed bagasse;
step two: soaking puffed bagasse in 12 times volume of enzyme solution, and hydrolyzing at 90-100 deg.C and pH of 4-5 for 20 min;
step three: adding trace C60 into the solution, treating the solution with ultrasonic wave with frequency of 28KHz for 35min, filtering, and collecting filtrate;
step four: adding ethanol to make the concentration of the ethanol in the filtrate reach 85%, precipitating bagasse polysaccharide solid, and vacuum drying to obtain bagasse polysaccharide solid;
step five: putting the bagasse polysaccharide solid into a carbonization furnace, naturally laying the raw material on a plane, raising the temperature to a carbonization temperature, and carbonizing to obtain the carbon molecular sieve;
step six: placing the carbon molecular sieve in a converter, heating to 950 ℃ under the protection of nitrogen, and introducing benzene to adjust the aperture of the carbon molecular sieve under the protection of nitrogen to obtain the nitrogen carbon molecular sieve;
the addition amount of the C60 is 0.05 percent of the weight of the bagasse;
the enzyme comprises cellulase, papain and pectinase;
the total weight of the enzyme is 0.1 percent of the weight of the bagasse, wherein the weight of the cellulase is 0.04 percent of the weight of the bagasse, the weight of the papain is 0.04 percent of the weight of the bagasse, and the weight of the pectinase is 0.02 percent of the weight of the bagasse;
the carbonization temperature is 980 ℃.
Example 2:
a method for preparing a nitrogen carbon molecular sieve with high specific surface area from bagasse comprises the following steps:
the method comprises the following steps: simply cleaning bagasse, mechanically pulverizing to 1-3mm, heating to 260 deg.C with steam, maintaining for 2min, and instantaneously releasing pressure within 0.1s to swell cell wall fiber of bagasse to obtain puffed bagasse;
step two: soaking puffed bagasse in 10 times volume of enzyme solution, and hydrolyzing at 90 deg.C and pH of 4-5 for 25 min;
step three: adding trace C60 into the solution, treating the solution with 35KHz ultrasonic wave for 40min, filtering, and collecting filtrate;
step four: adding ethanol to make the concentration of the ethanol in the filtrate reach 90%, precipitating bagasse polysaccharide solid, and vacuum drying to obtain bagasse polysaccharide solid;
step five: putting the bagasse polysaccharide solid into a carbonization furnace, naturally laying the raw material on a plane, raising the temperature to a carbonization temperature, and carbonizing to obtain the carbon molecular sieve;
step six: and (3) placing the carbon molecular sieve in a converter, heating to 1000 ℃ under the protection of nitrogen, and introducing benzene to adjust the aperture of the carbon molecular sieve under the protection of nitrogen to obtain the nitrogen carbon molecular sieve.
The addition amount of the C60 is 0.03 percent of the weight of the bagasse;
the enzyme includes cellulase, papain and pectinase.
The total weight of the enzyme is 0.2 percent of the weight of the bagasse, wherein the weight of the cellulase is 0.05 percent of the weight of the bagasse, the weight of the papain is 0.1 percent of the weight of the bagasse, and the weight of the pectinase is 0.05 percent of the weight of the bagasse.
The carbonization temperature is 950 ℃.
Example 3:
a method for preparing a nitrogen carbon molecular sieve with high specific surface area from bagasse comprises the following steps:
the method comprises the following steps: simply cleaning bagasse, mechanically pulverizing to 1-3mm, heating to 190 deg.C with steam, maintaining for 5min, and instantly releasing pressure within 1s to swell cell wall fiber of bagasse to obtain swelled bagasse;
step two: soaking puffed bagasse in 10 times volume of enzyme solution, and hydrolyzing at 90 deg.C and pH of 4-5 for 15 min;
step three: adding trace C60 into the solution, treating the solution with 25KHz ultrasonic wave for 40min, filtering, and collecting filtrate;
step four: adding ethanol to make the concentration of the ethanol in the filtrate reach 80%, precipitating bagasse polysaccharide solid, and vacuum drying to obtain bagasse polysaccharide solid;
step five: and putting the bagasse polysaccharide solid into a carbonization furnace, naturally laying the raw material on a plane, raising the temperature to a carbonization temperature, and carbonizing to obtain the carbon molecular sieve.
Step six: and (3) placing the carbon molecular sieve in a converter, heating to 970 ℃ under the protection of nitrogen, and introducing benzene to adjust the aperture of the carbon molecular sieve under the protection of nitrogen to obtain the nitrogen carbon molecular sieve.
The addition amount of C60 is 0.08% of the weight of bagasse
The enzyme includes cellulase, papain and pectinase.
The total weight of the enzyme is 0.05 percent of the weight of the bagasse, wherein the weight of the cellulase is 0.03 percent of the weight of the bagasse, the weight of the papain is 0.01 percent of the weight of the bagasse, and the weight of the pectinase is 0.01 percent of the weight of the bagasse.
The carbonization temperature is 1000 ℃.
Comparative example 1
The test data for the specific surface area of the molecular sieve obtained after carbonization by removing C60 in example 1 and keeping the other preparation conditions unchanged are as follows:
from the above test data, it can be seen that the addition of C60 has a very large effect on the specific surface area of the molecular sieve of the present invention.
The above embodiments are only preferred embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the scope of the present invention, and all equivalent substitutions or changes according to the technical solutions and the inventive concepts of the present invention should be covered by the scope of the present invention.
Claims (1)
1. A method for preparing a nitrogen carbon molecular sieve with high specific surface area from bagasse is characterized by comprising the following steps:
the method comprises the following steps: simply cleaning bagasse, mechanically pulverizing the bagasse into 1-3mm, heating to 190 ℃ by steam, maintaining for 5min, and instantly releasing pressure within 1s to swell cell wall fibers of the bagasse to obtain swelled bagasse for later use;
step two: soaking puffed bagasse in 10 times volume of enzyme solution, and hydrolyzing at 90 deg.C and pH of 4-5 for 15 min;
step three: adding trace C60 into the solution, treating the solution with 25KHz ultrasonic wave for 40min, filtering, and collecting filtrate;
step four: adding ethanol to make the concentration of the ethanol in the filtrate reach 80%, precipitating bagasse polysaccharide solid, and vacuum drying to obtain bagasse polysaccharide solid;
step five: putting the bagasse polysaccharide solid into a carbonization furnace, naturally laying the raw material on a plane, raising the temperature to the carbonization temperature, and carbonizing to obtain the carbon molecular sieve;
step six: placing the carbon molecular sieve in a converter, heating to 970 ℃ under the protection of nitrogen, and introducing benzene to adjust the aperture of the carbon molecular sieve under the protection of nitrogen to obtain the nitrogen carbon molecular sieve;
the addition amount of the C60 is 0.08 percent of the weight of the bagasse;
the enzyme comprises cellulase, papain and pectinase;
the total weight of the enzyme is 0.05 percent of the weight of the bagasse, wherein the weight of the cellulase is 0.03 percent of the weight of the bagasse, the weight of the papain is 0.01 percent of the weight of the bagasse, and the weight of the pectinase is 0.01 percent of the weight of the bagasse;
the carbonization temperature is 1000 ℃.
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| CN201710903171.9A CN107555432B (en) | 2016-07-09 | 2016-07-09 | Method for preparing nitrogen carbon molecular sieve with high specific surface area from bagasse |
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| 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 |
| CN201710903171.9A CN107555432B (en) | 2016-07-09 | 2016-07-09 | Method for preparing nitrogen carbon molecular sieve with high specific surface area from bagasse |
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| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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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| 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 |
| 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 |
| 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 |
| 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 |
| 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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| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1472134A (en) * | 2003-06-05 | 2004-02-04 | 上海交通大学 | Method for preparing carbon molecular sieve from apple dregs |
| CN101171956A (en) * | 2007-11-27 | 2008-05-07 | 南方医科大学 | Method for extracting polyoses from bagasse |
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| CN103435819B (en) * | 2013-07-17 | 2015-04-15 | 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 |
| 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 CN201610537404.3A patent/CN106185916B/en active Active
- 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 CN201710903084.3A patent/CN107585766A/en not_active Withdrawn
- 2016-07-09 CN CN201710903089.6A patent/CN107792852A/en not_active Withdrawn
- 2016-07-09 CN CN201710903083.9A patent/CN107572516A/en not_active Withdrawn
- 2016-07-09 CN CN201710903175.7A patent/CN107619048A/en not_active Withdrawn
- 2016-07-09 CN CN201710903174.2A patent/CN107673349A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1472134A (en) * | 2003-06-05 | 2004-02-04 | 上海交通大学 | Method for preparing carbon molecular sieve from apple dregs |
| CN1202992C (en) * | 2003-06-05 | 2005-05-25 | 上海交通大学 | Method for preparing carbon molecular sieve from apple dregs |
| CN101171956A (en) * | 2007-11-27 | 2008-05-07 | 南方医科大学 | Method for extracting polyoses from bagasse |
| CN101171956B (en) * | 2007-11-27 | 2010-07-21 | 南方医科大学 | Method for extracting polyoses from bagasse |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107585766A (en) | 2018-01-16 |
| CN107572516A (en) | 2018-01-12 |
| CN106185916B (en) | 2017-12-26 |
| CN106185916A (en) | 2016-12-07 |
| CN107673349A (en) | 2018-02-09 |
| CN107777684A (en) | 2018-03-09 |
| CN107619048A (en) | 2018-01-23 |
| CN107792852A (en) | 2018-03-13 |
| CN107555432A (en) | 2018-01-09 |
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