CN102583367A - Preparation technology of mesopore-rich active carbon with high specific surface area - Google Patents

Preparation technology of mesopore-rich active carbon with high specific surface area Download PDF

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Publication number
CN102583367A
CN102583367A CN2012100261981A CN201210026198A CN102583367A CN 102583367 A CN102583367 A CN 102583367A CN 2012100261981 A CN2012100261981 A CN 2012100261981A CN 201210026198 A CN201210026198 A CN 201210026198A CN 102583367 A CN102583367 A CN 102583367A
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Prior art keywords
room temperature
koh
surface area
naoh
specific surface
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CN2012100261981A
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Chinese (zh)
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李开喜
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Shanxi Institute of Coal Chemistry of CAS
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Shanxi Institute of Coal Chemistry of CAS
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Abstract

The invention relates to a preparation technology of mesopore-rich active carbon with high specific surface area. The preparation technology comprises the following steps of: uniformly mixing carbon-containing precursor with KOH or NaOH according to the weight ratio of carbon-containing precursor to KOH or NaOH of 1:(3-6), rising the room temperature to 800-1000 DEG C, maintaining constant temperature for 1-3 hours, then naturally reducing the temperature to room temperature, taking out an activated product, cleaning the activated product to be neutral with a great amount of water, mixing the activated product with the KOH or NaOH according to the weight ratio of 1:(1-3), rising the room temperature to 800-1000 DEG C, maintaining constant temperature for 1-3 hours, then naturally reducing the temperature to room temperature, cleaning the activated product to be neutral with water, drying and obtaining a product. The method has the advantages that the cleaned waste alkali can be recycled, the environmental-protection pressure is relieved, the production cost is reduced, the specific surface area is high, the aperture of mesopores is larger, the mesopores are rich, and no metal catalyst remains.

Description

A kind of technology of preparing that is rich in the mesopore active carbon with high specific surface area
Technical field
The invention belongs to a kind of technology of preparing that gac is provided, relate to a kind of technology of preparing that is rich in the mesopore active carbon with high specific surface area specifically.
Background technology
Be rich in the technology of preparing of the active carbon with high specific surface area of mesopore, provide a kind of charcoal precursor that contains specifically and successively carry out the method for chemical activation, so that make the active carbon with high specific surface area that is rich in mesopore with KOH and NaOH.
Patent CN201110103034.X " utilizes linters to prepare the method for active carbon with high specific surface area fiber " linters is placed fermentor tank, inoculation variable color pore fungus or whiterot fungi, and fermentative processing is washed once more, is dried; KOH or NaOH are put into reaction kettle to carry out activation and makes gac;
Patent CN201010177879.9 " a kind of microwave complex activation method for preparing super porous carbon " is a raw material with the mixture of petrochemical industry class carbon containing thing and plant class carbon containing thing, adds KOH/NaOH composite activating agent and iron/cobalt/nickel catalyzator again, obtains gac; Similarly patent CN200510025515.8 " a kind of preparation method who is rich in the mesopore active carbon with high specific surface area " is to be raw material with the petroleum coke powder, when adopting KOH aqueous solution dipping, adds soluble metallic salt and obtains mesopore.The problem of these two patents is that the metal catalyst that remains on the gac is difficult for removing, and influences the performance and the application of gac;
Patent CN200610041562.6 " a kind of method for preparing the abundant active carbon with high specific surface area of mesopore " carries out activation with KOH preparation back to containing carbon matrix precursor by a certain percentage with NaOH; Though the gac that had not only been contained mesopore but also had high specific surface area easily; But complicated component in the salkali waste that thick product washing back produces after the activation; Can't separate, be difficult for recycle;
Patent ZL200410012345 " a kind of preparation method of high-specific surface area mesopore charcoal " is the re-activation that gac is carried out KOH, and the mesopore aperture of gained gac is less relatively, and aperture control is difficult, influences its use range.
Summary of the invention
The purpose of this invention is to provide that a kind of scrub raffinate reusable edible, mesopore aperture are big, the residual technology of preparing that is rich in the mesopore active carbon with high specific surface area of non-metallic ion.
Concrete technology of preparing of the present invention is following:
By the weight ratio that contains carbon precursor and KOH or NaOH is 1: (3-6); To contain carbon precursor and KOH or NaOH and mix the back and be raised to 800-1000 ℃ from room temperature, and cool to room temperature naturally after constant temperature 1-3 hour, taking-up is after activation products wash neutrality with massive laundering; Weight ratio by activation products and KOH or NaOH is 1: (1-3); Activation products with after KOH or NaOH mix, are raised to 800-1000 ℃ from room temperature again, cool to room temperature naturally after constant temperature 1-3 hour; Water is drying to obtain product after activation products are washed neutrality.
The aforesaid carbon precursor that contains is refinery coke, coal, resol, corn straw, shell carbonized material, bamboo charcoal, coconut husk carbonized material, charred rice husk material.
Advantage of the present invention:
1, KOH and NaOH divide and to open use, can reclaim the salkali waste after the washing respectively, are convenient to the recycle of salkali waste, and alleviate environmental protection pressure, reduce production costs;
2, the product for preparing of this technology had both contained high specific surface area, be rich in certain mesopore again simultaneously, and non-metal catalyst was residual;
3, the mesopore aperture of this technology products obtained therefrom is prone to control, and pore size can be through KOH and NaOH regulation and control.
4, the mesopore aperture of this technology products obtained therefrom is bigger.
Embodiment
Embodiment 1
The aforesaid carbon precursor that contains is refinery coke, coal, resol, corn straw carbonized material, shell carbonized material, bamboo charcoal, coconut husk carbonized material, charred rice husk material.
With weight ratio is that 1: 3 refinery coke and KOH mixes the back and be raised to 1000 ℃ from room temperature; Constant temperature cools to room temperature naturally after 3 hours, take out after activation products wash neutrality with massive laundering, according to activation products with after the weight ratio of NaOH is mixed at 1: 3; Be raised to 800 ℃ from room temperature again; Constant temperature cools to room temperature naturally after 1 hour, with big water gaging activation products are washed neutrality after, be drying to obtain product.The specific surface area of gained gac is 2602m2/g, and the mesopore aperture concentrates on the 5-8nm scope, and middle porosity is up to 65%.
Embodiment 2
With weight ratio is that 1: 6 Yangquan hard coal and KOH mixes the back and be raised to 800 ℃ from room temperature; Constant temperature cools to room temperature naturally after 1 hour, take out after activation products wash neutrality with massive laundering, according to activation products with after the weight ratio of NaOH is mixed at 1: 1; Be raised to 1000 ℃ from room temperature again; Constant temperature cools to room temperature naturally after 1 hour, with big water gaging activation products are washed neutrality after, be drying to obtain product.The specific surface area of gained gac is 2958m2/g, and the mesopore aperture concentrates on the 4-6nm scope, and middle porosity is up to 58%.
Embodiment 3
With weight ratio is that 1: 4 bamboo charcoal and KOH mixes the back and be raised to 900 ℃ from room temperature; Constant temperature cools to room temperature naturally after 2 hours, take out after activation products wash neutrality with massive laundering, according to activation products with after the weight ratio of NaOH is mixed at 1: 2; Be raised to 800 ℃ from room temperature again; Constant temperature cools to room temperature naturally after 3 hours, with big water gaging activation products are washed neutrality after, be drying to obtain product.The specific surface area of gained gac is 2359m2/g, and the mesopore aperture concentrates on the 3-6nm scope, middle porosity 60%.
Embodiment 4
With weight ratio is that 1: 6 resol and NaOH mixes the back and be raised to 800 ℃ from room temperature; Constant temperature cools to room temperature naturally after 3 hours, take out after activation products wash neutrality with massive laundering, according to activation products with after the weight ratio of KOH is mixed at 1: 1; Be raised to 800 ℃ from room temperature again; Constant temperature cools to room temperature naturally after 3 hours, with big water gaging activation products are washed neutrality after, be drying to obtain product.The specific surface area of gained gac is 2100m2/g, and the mesopore aperture concentrates on the 3-5nm scope, middle porosity 38%.
Embodiment 5
With weight ratio is that 1: 5 corn straw carbonized material and NaOH mixes the back and be raised to 800 ℃ from room temperature; Constant temperature cools to room temperature naturally after 1 hour, take out after activation products wash neutrality with massive laundering, according to activation products with after the weight ratio of KOH is mixed at 1: 3; Be raised to 800 ℃ from room temperature again; Constant temperature cools to room temperature naturally after 2 hours, with big water gaging activation products are washed neutrality after, be drying to obtain product.The specific surface area of gained gac is 2345m2/g, and the mesopore aperture concentrates on the 5-8nm scope, and middle porosity is up to 40%.
Embodiment 6
With weight ratio is that 1: 3 shell carbonized material and NaOH mixes the back and be raised to 1000 ℃ from room temperature; Constant temperature cools to room temperature naturally after 3 hours, take out after activation products wash neutrality with massive laundering, according to activation products with after the weight ratio of KOH is mixed at 1: 1; Be raised to 1000 ℃ from room temperature again; Constant temperature cools to room temperature naturally after 3 hours, with big water gaging activation products are washed neutrality after, be drying to obtain product.The specific surface area of gained gac is 2532m2/g, and the mesopore aperture concentrates on the 6-8nm scope, middle porosity 51%.
Embodiment 7
With weight ratio is that 1: 4 coconut husk carbonized material and NaOH mixes the back and be raised to 900 ℃ from room temperature; Constant temperature cools to room temperature naturally after 1 hour, take out after activation products wash neutrality with massive laundering, according to activation products with after the weight ratio of KOH is mixed at 1: 2; Be raised to 900 ℃ from room temperature again; Constant temperature cools to room temperature naturally after 3 hours, with big water gaging activation products are washed neutrality after, be drying to obtain product.The specific surface area of gained gac is 2412m2/g, and the mesopore aperture concentrates on the 4-6nm scope, and middle porosity is up to 44%.
Embodiment 8
With weight ratio is that 1: 5 charred rice husk material and NaOH mixes the back and be raised to 800 ℃ from room temperature; Constant temperature cools to room temperature naturally after 3 hours, take out after activation products wash neutrality with massive laundering, according to activation products with after the weight ratio of KOH is mixed at 1: 2; Be raised to 800 ℃ from room temperature again; Constant temperature cools to room temperature naturally after 3 hours, with big water gaging activation products are washed neutrality after, be drying to obtain product.The specific surface area of gained gac is 2012m2/g, and the mesopore aperture concentrates on the 3-5nm scope, and middle porosity is up to 33%.

Claims (2)

1. a technology of preparing that is rich in the mesopore active carbon with high specific surface area is characterized in that comprising the steps:
By the weight ratio that contains carbon precursor and KOH or NaOH is 1: 3-6, and will contain carbon precursor and KOH or NaOH and mix, be raised to 800-1000 ℃ from room temperature; Naturally cool to room temperature after constant temperature 1-3 hour; Taking out activation products and wash neutrality with massive laundering, is 1 by the weight ratio of activation products and KOH or NaOH: 1-3, with activation products with after KOH or NaOH mix; Be raised to 800-1000 ℃ from room temperature again; Naturally cool to room temperature after constant temperature 1-3 hour, water washs neutrality with activation products, is drying to obtain product.
2. a kind of technology of preparing that is rich in the mesopore active carbon with high specific surface area as claimed in claim 1 is characterized in that the described carbon precursor that contains is refinery coke, coal, resol, corn straw, shell carbonized material, bamboo charcoal, coconut husk carbonized material or charred rice husk material.
CN2012100261981A 2012-01-19 2012-01-19 Preparation technology of mesopore-rich active carbon with high specific surface area Pending CN102583367A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103887033A (en) * 2014-03-13 2014-06-25 常州中科海纳碳素科技有限公司 Method for preparing activated carbon capable of absorbing electromagnetic waves
CN104307523A (en) * 2014-09-18 2015-01-28 四川大学 One-step method for preparation of iron loaded activated carbon catalyst from rice husk pyrolytic carbon
CN106517183A (en) * 2016-11-15 2017-03-22 河南理工大学 A low-cost simple preparing method for nitrogen-doped porous charcoal with a high specific surface area
CN107311171A (en) * 2017-07-11 2017-11-03 吉林大学 The preparation method and activated carbon of activated carbon
CN107500291A (en) * 2017-07-10 2017-12-22 吉林大学 A kind of preparation method of lignin-base phenolic resin capacitance carbon
CN108378063A (en) * 2018-05-18 2018-08-10 中国农业科学院农业环境与可持续发展研究所 A kind of preparation method of muscardine granule
CN109384229A (en) * 2018-09-29 2019-02-26 中国科学院山西煤炭化学研究所 It is a kind of towards the high-energy-density supercapacitor preparation method of phosphorus doping porous carbon electrode material
CN111689495A (en) * 2020-05-15 2020-09-22 内蒙古浦瑞芬环保科技有限公司 Preparation method of tar-free activated carbon
CN111715185A (en) * 2020-06-16 2020-09-29 中国环境科学研究院 Biochar-based adsorbent for removing organic pollutants in sewage
CN113135567A (en) * 2021-04-28 2021-07-20 安徽工程大学 Preparation method of activated carbon and product thereof

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CN1927708A (en) * 2006-09-15 2007-03-14 江苏工业学院 Method of preparing high specific surface area activated carbon with rich mesoporous

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103887033A (en) * 2014-03-13 2014-06-25 常州中科海纳碳素科技有限公司 Method for preparing activated carbon capable of absorbing electromagnetic waves
CN104307523A (en) * 2014-09-18 2015-01-28 四川大学 One-step method for preparation of iron loaded activated carbon catalyst from rice husk pyrolytic carbon
CN104307523B (en) * 2014-09-18 2016-03-30 四川大学 A kind of method being prepared year Fischer-Tropsch synthesis by rice husk thermal decomposition charcoal one step
CN106517183A (en) * 2016-11-15 2017-03-22 河南理工大学 A low-cost simple preparing method for nitrogen-doped porous charcoal with a high specific surface area
CN107500291A (en) * 2017-07-10 2017-12-22 吉林大学 A kind of preparation method of lignin-base phenolic resin capacitance carbon
CN107500291B (en) * 2017-07-10 2019-10-18 吉林大学 A kind of preparation method of lignin-base phenolic resin capacitance carbon
CN107311171A (en) * 2017-07-11 2017-11-03 吉林大学 The preparation method and activated carbon of activated carbon
CN108378063A (en) * 2018-05-18 2018-08-10 中国农业科学院农业环境与可持续发展研究所 A kind of preparation method of muscardine granule
CN109384229A (en) * 2018-09-29 2019-02-26 中国科学院山西煤炭化学研究所 It is a kind of towards the high-energy-density supercapacitor preparation method of phosphorus doping porous carbon electrode material
CN111689495A (en) * 2020-05-15 2020-09-22 内蒙古浦瑞芬环保科技有限公司 Preparation method of tar-free activated carbon
CN111715185A (en) * 2020-06-16 2020-09-29 中国环境科学研究院 Biochar-based adsorbent for removing organic pollutants in sewage
CN113135567A (en) * 2021-04-28 2021-07-20 安徽工程大学 Preparation method of activated carbon and product thereof

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Application publication date: 20120718