CN112456469A - Method for preparing nano-graded porous carbon material based on rice hull ash - Google Patents
Method for preparing nano-graded porous carbon material based on rice hull ash Download PDFInfo
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- CN112456469A CN112456469A CN202110061886.0A CN202110061886A CN112456469A CN 112456469 A CN112456469 A CN 112456469A CN 202110061886 A CN202110061886 A CN 202110061886A CN 112456469 A CN112456469 A CN 112456469A
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Abstract
The invention provides a method for preparing a nano graded porous carbon material based on rice hull ash, and relates to the technical field of nano carbon. The method comprises the following steps: preparing raw materials, namely grinding and crushing the rice hull ash, adding a proper amount of caustic soda, and directly generating a mixture of liquid water glass and the rice hull ash in a high-pressure steamer, wherein the step two comprises the following steps: pretreating raw materials, and reacting the mixture of rice husk ash and water glass with tellurium tetrafluoride in a reaction kettle. Through silica and caustic soda production water glass to rice husk ash contains, adopt tellurium tetrafluoride to mix production silicon tetrafluoride afterwards, can improve the evaporation of temperature stabilization, the easier separates silica, avoid reducing the unit surface area of rice husk ash because silica, secondly through avoiding using hydrofluoric acid, other types of strong base and strong acid, can guarantee the security to the rice husk ash, avoid producing the staff that strong acid and strong base hurt the production, improve the efficiency of production in step, simplify the production step.
Description
Technical Field
The invention relates to the technical field of nano carbon, in particular to a method for preparing a nano graded porous carbon material based on rice hull ash.
Background
The nano carbon material is a carbon material with at least one dimension of a disperse phase dimension less than 100 nanometers. The dispersed phase may consist of carbon atoms, may also consist of heterogeneous atoms (non-carbon atoms), and may even be nanoporous. The nano carbon material mainly comprises three types of carbon nano tubes, carbon nano fibers and nano carbon spheres.
At present, most of the used nano carbon materials are purified by removing impurities by using clean carbon materials, in the actual production process, because rice hulls contain a large amount of lignin and cellulose, the raw materials for preparing nano carbon have better performance, but after the results are burnt, about 1.3 percent of silicide can be mixed in rice hull ash, if the silicide is not treated, the unit surface area of the nano carbon can be reduced in the subsequent preparation process, but most of the existing treatment modes adopt hydrofluoric acid and various types of strong acid and strong base for removal, in the actual removal process, the actual removal efficiency of the silicon compound is not good, new impurities are often generated and mixed in the rice hull ash, and then the strong acid and the strong base are adopted, so that the production process is complicated, the production efficiency is not improved for users, and once the strong acid and the strong base are leaked, the serious safety production accident is easy to produce, and the serious accident of personal injury is caused.
Disclosure of Invention
The invention aims to provide a method for preparing a nano-graded porous carbon material based on rice hull ash. Through silica and caustic soda production water glass to rice husk ash contains, adopt tellurium tetrafluoride to mix production silicon tetrafluoride afterwards, can improve the evaporation of temperature stabilization, it separates silica more easily, avoid because silica reduces the unit surface area of rice husk ash, improve the competitive edge of material, secondly through avoiding using hydrofluoric acid, other types of strong base and strong acid, can guarantee the security to the rice husk ash, avoid producing the staff that strong acid and strong base hurt the production, improve the efficiency of production in step, simplify the production step.
In order to solve the problems of poor environment-friendly performance and low structural strength, the invention provides the following technical scheme: a method for preparing a nano-graded porous carbon material based on rice hull ash comprises the following steps:
the method comprises the following steps: the preparation of raw materials comprises the steps of grinding and crushing the rice hull ash, adding a proper amount of caustic soda, and directly generating a mixture of liquid water glass and the rice hull ash in a high-pressure steamer.
Step two: the method comprises the following steps of raw material pretreatment, reaction of a mixture of rice husk ash and water glass and tellurium tetrafluoride in a reaction kettle, vacuumizing the reaction kettle in advance, and then hermetically conveying the mixture in the reaction kettle to a sealed evaporation vessel.
Step three: the preparation reaction comprises the steps of heating an evaporation vessel, cooling and taking out, mixing the rice hull ash and the shell nano carbon powder, injecting a small amount of dilute hydrochloric acid for mixing and soaking, then cleaning with ionized water, distilling, roughly cleaning and airing.
Step four: and (3) product treatment, namely placing the rice hull ash in a tubular furnace under inert gas for activation treatment, and then taking out, sealing and cooling.
Further, the method comprises the following steps: according to the operation steps in the step one, a grinding device adopted by the rice hull ash needs to use a rotating speed of 500 revolutions per minute to grind the rice hull ash for thirty minutes, and a proper amount of caustic soda is additionally added for fifteen minutes after grinding.
Further, the method comprises the following steps: according to the operation steps in the first step, the working temperature of the high-pressure steamer is 0.6-1.0 MPa steam for reaction.
Further, the method comprises the following steps: according to the operation steps in the second step, before the mixture of the rice hull ash and the water glass reacts with the tellurium tetrafluoride, a proper amount of dilute hydrochloric acid is added into the mixture of the rice hull ash and the water glass, and the mixture is kept stand, precipitated and dehydrated.
Further, the method comprises the following steps: according to the operation steps in the second step, after the interior of the reaction kettle is vacuumized, a part of appropriate inert gas is additionally added.
Further, the method comprises the following steps: according to the operation steps in the second step, the mixture of the rice hull ash and the water glass reacts with tellurium tetrafluoride in a reaction kettle, sufficient silicon tetrafluoride is generated, the boiling point of the silicon tetrafluoride is-65 ℃, the working stability of the sealed evaporating dish is 15 ℃, and the silicon tetrafluoride is cooled, liquefied and collected by liquid nitrogen.
Further, the method comprises the following steps: according to the operation steps in the third step, the molar mass ratio of the shell nano carbon powder to the rice hull ash is 10: 1.
further, the method comprises the following steps: according to the operation steps in the third step, the rice hull ash and the shell nano carbon powder are soaked by the dilute hydrochloric acid, the soaking time is 1 hour, and the concentration of the dilute hydrochloric acid is 10 percent.
Further, the method comprises the following steps: according to the operation steps in the fourth step, the working temperature of the tube furnace is 890 ℃, the tube furnace needs to be preheated to 120 ℃ in advance before activation, after 10 minutes, the tube furnace adopts the speed of 10 ℃ rise in no minutes, the temperature is increased to 890 ℃, and the temperature lasts for 30 minutes at 890 ℃.
Further, the method comprises the following steps: according to the operation steps in the fourth step, sufficient potassium hydroxide is mixed during activation, and the potassium hydroxide is sealed and cooled by nitrogen protection, so that the potassium hydroxide is not in contact with external oxygen for cooling.
The invention provides a method for preparing a nano graded porous carbon material based on rice hull ash, which has the following beneficial effects: through silica and caustic soda production water glass to rice husk ash contains, adopt tellurium tetrafluoride to mix production silicon tetrafluoride afterwards, can improve the evaporation of temperature stabilization, it separates silica more easily, avoid because silica reduces the unit surface area of rice husk ash, improve the competitive edge of material, secondly through avoiding using hydrofluoric acid, other types of strong base and strong acid, can guarantee the security to the rice husk ash, avoid producing the staff that strong acid and strong base hurt the production, improve the efficiency of production in step, simplify the production step.
Drawings
Fig. 1 is a flow chart of a method for preparing a nano-sized porous carbon material based on rice hull ash according to the present invention.
Detailed Description
Referring to fig. 1, the present invention provides a technical solution: a method for preparing a nano-graded porous carbon material based on rice hull ash comprises the following steps:
the method comprises the following steps: the preparation of raw materials comprises the steps of grinding and crushing the rice hull ash, adding a proper amount of caustic soda, and directly generating a mixture of liquid water glass and the rice hull ash in a high-pressure steamer.
Step two: the method comprises the following steps of raw material pretreatment, reaction of a mixture of rice husk ash and water glass and tellurium tetrafluoride in a reaction kettle, vacuumizing the reaction kettle in advance, and then hermetically conveying the mixture in the reaction kettle to a sealed evaporation vessel.
Step three: the preparation reaction comprises the steps of heating an evaporation vessel, cooling and taking out, mixing the rice hull ash and the shell nano carbon powder, injecting a small amount of dilute hydrochloric acid for mixing and soaking, then cleaning with ionized water, distilling, roughly cleaning and airing.
Step four: and (3) product treatment, namely placing the rice hull ash in a tubular furnace under inert gas for activation treatment, and then taking out, sealing and cooling.
Specifically, the method comprises the following steps: according to the operation steps in the step one, a grinding device adopted by the rice hull ash needs to use a rotating speed of 500 revolutions per minute to grind the rice hull ash for thirty minutes, and a proper amount of caustic soda is additionally added after fifteen minutes of grinding.
Specifically, the method comprises the following steps: according to the operation steps in the first step, the working temperature of the high-pressure steamer is 0.6-1.0 MPa steam for reaction.
Specifically, the method comprises the following steps: according to the operation steps in the second step, before the mixture of the rice hull ash and the water glass reacts with the tellurium tetrafluoride, a proper amount of dilute hydrochloric acid is added into the mixture of the rice hull ash and the water glass, and the mixture is kept stand, precipitated and dehydrated.
Specifically, the method comprises the following steps: according to the operation steps in the second step, after the interior of the reaction kettle is vacuumized, a part of proper amount of inert gas is additionally added.
Specifically, the method comprises the following steps: according to the operation steps in the second step, the mixture of the rice hull ash and the water glass reacts with tellurium tetrafluoride in a reaction kettle to generate sufficient silicon tetrafluoride, the boiling point of the silicon tetrafluoride is-65 ℃, the work stability of a sealed evaporating dish is 15 ℃, and the silicon tetrafluoride is cooled, liquefied and collected by liquid nitrogen.
Specifically, the method comprises the following steps: according to the operation steps in the third step, the molar mass ratio of the shell nano carbon powder to the rice hull ash is 10: 1.
specifically, the method comprises the following steps: according to the operation steps in the third step, the rice hull ash and the shell nano carbon powder are soaked in the dilute hydrochloric acid for 1 hour, and the concentration of the dilute hydrochloric acid is 10 percent.
Specifically, the method comprises the following steps: according to the operation steps in the fourth step, the working temperature of the tube furnace is 890 ℃, the tube furnace needs to be preheated to 120 ℃ in advance before activation, after 10 minutes, the tube furnace adopts the speed of 10 ℃ rise in no minutes, the temperature is increased to 890 ℃, and the temperature lasts for 30 minutes at 890 ℃.
Specifically, the method comprises the following steps: according to the operation steps in the fourth step, during activation, sufficient potassium hydroxide is mixed, sealed cooling is carried out, nitrogen protection cooling needs to be carried out on the potassium hydroxide, and cooling without contact with external oxygen is guaranteed.
The method of the examples was performed for detection analysis and compared to the prior art to yield the following data:
| unit surface area | Production efficiency | |
| Examples | Is larger | Is higher than |
| Prior Art | Is smaller | Is lower than |
From the above table data, it can be concluded that, when the examples are used, the unit surface area of the product is further increased, the production efficiency and safety of the product are improved, and the overall production efficiency is improved by the method of preparing the nano-graded porous carbon material based on rice hull ash.
The invention provides a method for preparing a nano-graded porous carbon material based on rice hull ash, which comprises the following steps: the method comprises the following steps: raw material preparation, firstly, rice hull ash is ground and crushed, then, a proper amount of caustic soda is added, then, in a high-pressure steamer, a mixture of liquid water glass and rice hull ash is directly generated, a grinding device adopted by the rice hull ash needs to use the rotating speed of 500 rpm, the rice hull ash is ground for thirty minutes, fifteen minutes after grinding, a proper amount of caustic soda is additionally added, the working temperature of the high-pressure steamer is equal to and reacts under the steam of 0.6-1.0 MPa, through the caustic soda, in the high-pressure steamer of a wet method, silica can be converted into water glass, through grinding, the particle diameters of the rice hull ash and the silica can be further reduced, the effective area is improved, then, the reaction efficiency is conveniently improved, and through crushing of the caustic soda, the efficiency of the water glass of a support can also be improved, and the step two: pretreating raw materials, reacting a mixture of rice hull ash and water glass with tellurium tetrafluoride in a reaction kettle, vacuumizing the reaction kettle in advance, sealing and conveying the mixture in the reaction kettle into a sealed evaporation vessel, adding a proper amount of dilute hydrochloric acid into the mixture of the rice hull ash and the water glass before the mixture reacts with the tellurium tetrafluoride, standing, precipitating and dehydrating, adding a part of a proper amount of inert gas after vacuumizing the interior of the reaction kettle, reacting the mixture of the rice hull ash and the water glass with the tellurium tetrafluoride in the reaction kettle to generate a sufficient amount of silicon tetrafluoride, wherein the boiling point of the silicon tetrafluoride is-65 ℃, the working stability of the sealed evaporation vessel is 15 ℃, the silicon tetrafluoride is liquefied and collected by cooling liquid nitrogen, and reacts with silica gel generated by the tellurium tetrafluoride and the water glass to produce gas silicon tetrafluoride, during the reaction, unnecessary telluride evaporates the discharge, through adding dilute hydrochloric acid in the net water glass, can assist and convert into silica gel, through silicon tetrafluoride, can realize taking out silicon ion, purifies the inside impurity of rice husk ash, through sealed evaporating dish, can separate silicon tetrafluoride and rice husk ash, realizes taking out the effect of silicon ion, step three: the preparation reaction, heating evaporating dish, cooling and taking out, mixing rice hull ash and shell nano carbon powder, injecting a small amount of dilute hydrochloric acid for mixing and soaking, then adopting ionized water for cleaning, distilling, roughly washing and airing, wherein the molar mass ratio of the shell nano carbon powder to the rice hull ash is 10: 1, dilute hydrochloric acid soaks rice husk ash and shell nanometer carbon powder, and the time of soaking is 1 hour, and the concentration of dilute hydrochloric acid is 10%, through adding shell nanometer carbon powder, can realize improving the not enough condition of unit surface area of rice husk ash, avoids because fibre and lignin take place to decompose, the problem that the rice husk ash unit surface area that leads to descends, step four: product processing, with rice husk ash under inert gas, arrange the tube furnace in, carry out activation treatment, take out sealed cooling after afterwards, the operating temperature of tube furnace is 890 degrees centigrade, before the activation, need preheat to 120 degrees centigrade in advance, through preheating, can realize further taking place to sublime to the telluride that contains in the rice husk ash, leave rice husk ash mixture, last 10 minutes back, the tube furnace adopts not minute the speed that rises 10 degrees centigrade, raise the temperature to 890 degrees centigrade, when lasting 890 degrees centigrade temperature 30 minutes activation, mix sufficient potassium hydroxide, sealed cooling, need carry out nitrogen protection cooling to it, guarantee not contact the cooling with external oxygen, through potassium hydroxide, can realize the further activation to rice husk ash and shell nanometer carbon powder.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A method for preparing a nano-graded porous carbon material based on rice hull ash is characterized by comprising the following steps:
the method comprises the following steps: preparing raw materials, namely grinding and crushing the rice hull ash, adding a proper amount of caustic soda, and directly generating a mixture of liquid water glass and the rice hull ash in a high-pressure steamer;
step two: pretreating raw materials, namely reacting a mixture of rice hull ash and water glass with tellurium tetrafluoride in a reaction kettle, vacuumizing the reaction kettle in advance, and then hermetically conveying the mixture in the reaction kettle to a sealed evaporation vessel;
step three: the preparation reaction comprises the steps of heating an evaporation vessel, cooling and taking out, mixing the rice hull ash and the shell nano carbon powder, injecting a small amount of dilute hydrochloric acid for mixing and soaking, then cleaning with ionized water, distilling, roughly cleaning and airing;
step four: and (3) product treatment, namely placing the rice hull ash in a tubular furnace under inert gas for activation treatment, and then taking out, sealing and cooling.
2. The method for preparing the nano-graded porous carbon material based on the rice hull ash according to claim 1, which comprises the following steps: according to the operation steps in the step one, a grinding device adopted by the rice hull ash needs to use a rotating speed of 500 revolutions per minute to grind the rice hull ash for thirty minutes, and a proper amount of caustic soda is additionally added for fifteen minutes after grinding.
3. The method for preparing the nano-graded porous carbon material based on the rice hull ash according to claim 1, which comprises the following steps: according to the operation steps in the first step, the working temperature of the high-pressure steamer is 0.6-1.0 MPa steam for reaction.
4. The method for preparing the nano-graded porous carbon material based on the rice hull ash according to claim 1, which comprises the following steps: according to the operation steps in the second step, before the mixture of the rice hull ash and the water glass reacts with the tellurium tetrafluoride, a proper amount of dilute hydrochloric acid is added into the mixture of the rice hull ash and the water glass, and the mixture is kept stand, precipitated and dehydrated.
5. The method for preparing the nano-graded porous carbon material based on the rice hull ash according to claim 1, which comprises the following steps: according to the operation steps in the second step, after the interior of the reaction kettle is vacuumized, a part of appropriate inert gas is additionally added.
6. The method for preparing the nano-graded porous carbon material based on the rice hull ash according to claim 1, which comprises the following steps: according to the operation steps in the second step, the mixture of the rice hull ash and the water glass reacts with tellurium tetrafluoride in a reaction kettle, sufficient silicon tetrafluoride is generated, the boiling point of the silicon tetrafluoride is-65 ℃, the working stability of the sealed evaporating dish is 15 ℃, and the silicon tetrafluoride is cooled, liquefied and collected by liquid nitrogen.
7. The method for preparing the nano-graded porous carbon material based on the rice hull ash according to claim 1, which comprises the following steps: according to the operation steps in the third step, the molar mass ratio of the shell nano carbon powder to the rice hull ash is 10: 1.
8. the method for preparing the nano-graded porous carbon material based on the rice hull ash according to claim 1, which comprises the following steps: according to the operation steps in the third step, the rice hull ash and the shell nano carbon powder are soaked by the dilute hydrochloric acid, the soaking time is 1 hour, and the concentration of the dilute hydrochloric acid is 10 percent.
9. The method for preparing the nano-graded porous carbon material based on the rice hull ash according to claim 1, which comprises the following steps: according to the operation steps in the fourth step, the working temperature of the tube furnace is 890 ℃, the tube furnace needs to be preheated to 120 ℃ in advance before activation, after 10 minutes, the tube furnace adopts the speed of 10 ℃ rise in no minutes, the temperature is increased to 890 ℃, and the temperature lasts for 30 minutes at 890 ℃.
10. The method for preparing the nano-graded porous carbon material based on the rice hull ash according to claim 1, which comprises the following steps: according to the operation steps in the fourth step, sufficient potassium hydroxide is mixed during activation, and the potassium hydroxide is sealed and cooled by nitrogen protection, so that the potassium hydroxide is not in contact with external oxygen for cooling.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039000A (en) * | 1988-06-30 | 1990-01-24 | 南京林业大学 | Rice hull ash coproduction water glass and gac |
| RU2002122453A (en) * | 2002-08-19 | 2004-02-27 | Федеральное государственное унитарное предпри тие "Сибирский химический комбинат" Министерства Российской Федерации по атомной энергии | Method for producing elemental tellurium |
| CN101704526A (en) * | 2009-10-13 | 2010-05-12 | 李洪锡 | Method for producing white carbon black and active carbon by using residual rice hull ash after gasification |
| KR20190002896A (en) * | 2017-06-30 | 2019-01-09 | 충남대학교산학협력단 | A porous carbon beads having hierarchical pore structure and the method for preparation thereof |
| WO2020150855A1 (en) * | 2019-01-21 | 2020-07-30 | 金华晨阳科技有限公司 | Hollow carbon sphere with multi-stage pore structure and preparation method therefor |
-
2021
- 2021-01-18 CN CN202110061886.0A patent/CN112456469A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039000A (en) * | 1988-06-30 | 1990-01-24 | 南京林业大学 | Rice hull ash coproduction water glass and gac |
| RU2002122453A (en) * | 2002-08-19 | 2004-02-27 | Федеральное государственное унитарное предпри тие "Сибирский химический комбинат" Министерства Российской Федерации по атомной энергии | Method for producing elemental tellurium |
| CN101704526A (en) * | 2009-10-13 | 2010-05-12 | 李洪锡 | Method for producing white carbon black and active carbon by using residual rice hull ash after gasification |
| KR20190002896A (en) * | 2017-06-30 | 2019-01-09 | 충남대학교산학협력단 | A porous carbon beads having hierarchical pore structure and the method for preparation thereof |
| WO2020150855A1 (en) * | 2019-01-21 | 2020-07-30 | 金华晨阳科技有限公司 | Hollow carbon sphere with multi-stage pore structure and preparation method therefor |
Non-Patent Citations (1)
| Title |
|---|
| 苏学军等: "稻壳基二氧化硅的制备及应用研究进展" * |
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