CN101816929B - Method for preparing imporous carbon absorbent material - Google Patents
Method for preparing imporous carbon absorbent material Download PDFInfo
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- CN101816929B CN101816929B CN2009101175036A CN200910117503A CN101816929B CN 101816929 B CN101816929 B CN 101816929B CN 2009101175036 A CN2009101175036 A CN 2009101175036A CN 200910117503 A CN200910117503 A CN 200910117503A CN 101816929 B CN101816929 B CN 101816929B
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Abstract
The invention discloses a method for preparing an imporous carbon absorbent material, which comprises the following steps of: firstly, taking sucrose, adding 98 percent sulfuric acid for carbonization in a mass ratio of 1:2-4 to obtain a carbon precursor; secondly, heating the carbon precursor to the temperature of between 150 and 180 DEG C, and pre-oxidizing the carbon precursor to a bread shape; thirdly, continuously oxidizing the product for 4 to 5 hours under the vacuum degree between 0.06 and 0.08MPa and at the temperature of between 220 and 230 DEG C, and absorbing the produced waste gas by using alkali liquor; and finally, performing vacuum cooling on the product to room temperature under the vacuum degree between 0.06 and 0.08Mpa, and grinding to obtain the novel imporous carbon absorbent material.
Description
Technical field
The present invention relates to the preparation method of carbon material adsorbing material.
Background technology
Since 18 end of the centurys, people found first that charcoal had adsorption capacity, carbon material adsorbing material such as active carbon, graphite and carbon black etc. have become a most widely used class sorbing material at present, be widely used in water treatment, air cleaning, catalyst cupport, decolouring, various fields such as precious metal recovery and electronics industry.Wherein activated carbon is the most frequently used a kind of sorbing material because of its abundant pore structure and great specific area have good adsorption capacity.Active carbon is by raw material unusual the non-renewable resources class that is divided into, renewable resource class and discarded object class.Non-renewable resources class active carbon such as various active carbon from coal, this class activity output maximum in all kinds of active carbons, but quality is often not high, and added value of product is lower, is mainly used in wastewater treatment, fields such as purification of water quality and decolouring.Renewable resource class active carbon such as activated carbon from bamboo, wood activated charcoal, this class active carbon quality is higher; be mainly used in air cleaning, fields such as precious metal recovery and electronics industry, added value of product height; but this type of active carbon is with trees, and plants such as bamboo are unfavorable for ecological protection as the charcoal source.Discarded object class active carbon serves as typical case's representative with cocoanut active charcoal and petroleum coke matrix activated carbon, and raw material sources are various, and quality is different according to the charcoal source.Though this class active carbon is turned waste into wealth, with changing rejected material to useful resource, source, single charcoal source is limited, is unfavorable for large-scale production.Active carbon needs high-temperature physics activation or chemical activation in preparation process, and needs cyclic washing, complicated process of preparation, and cost is higher, and Application of Brand Active Carbon is restricted.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of imporous carbon absorbent material.
The present invention is a kind of preparation method of imporous carbon absorbent material, the steps include:
(1) gets sucrose, add 98% sulfuric acid charing, get the carbonaceous presoma by mass ratio 1: 2~4;
(2) carbonaceous presoma in above-mentioned (1) is heated to 150~180 ℃, pre-oxidation is to bread-like;
(3) with product in above-mentioned (2) in vacuum 0.06~0.08Mpa, under 220~230 ℃ of the temperature, continue oxidation 4~5 hours, the waste gas that is produced absorbs with alkali lye;
(4) vacuum cooled under vacuum 0.06~0.08MPa of product in above-mentioned (3) is ground to room temperature, promptly obtain novel imporous carbon absorbent material.
The present invention has following advantage:
1, with sucrose is the charcoal source, belongs to renewable resource.
2, be carbonized agent with 98% sulfuric acid, carbonization temperature is a room temperature, and carbonization process need not high temperature, and 98% sulfuric acid is incomplete to the charing of sucrose, the part not sucrose molecule fragment of complete charing contains abundant oxygen-containing functional group, helps the generation of sorbing material surface-active adsorption site.
3, oxidizing process is utilized the oxidisability of the concentrated sulfuric acid self, need not oxidant applying; Oxidizing process is carried out under vacuum, helps protecting imporous carbon absorbent material, and it is not is not scattered and disappeared by calcination; Sulfuric acid evaporates automatically in the oxidizing process, and the sorbing material of preparation grinds the back and directly uses, and need not post processing and removes sulfuric acid; The waste gas that produces in the oxidizing process absorbs with alkali lye, environment is not worked the mischief.
4, prepared carbon material adsorbing material belongs to non-porous structure, and specific area is 0.6m only
2/ g, but the adsorption capacity of methylene blue is better than commercially available active carbon reaches 60~70% of commercially available active carbon to the adsorption capacity of Cr (VI), and alternative active carbon is used for the adsorption treatment of heavy metal ions in wastewater and organic dyestuff.
Description of drawings
Fig. 1 is the SEM figure of prepared imporous carbon absorbent material, Fig. 2 be prepared imporous carbon absorbent material and other materials to methylene blue adsorption effect comparison diagram, Fig. 3 is that prepared imporous carbon absorbent material and other materials are to Cr (VI) adsorption effect comparison diagram.
The specific embodiment
Embodiment 1:
Get sucrose, press mass ratio and add 98% sulfuric acid at 1: 2, stir, 150 ℃ of pre-oxidation are to bread-like, in vacuum 0.08Mpa, under 220 ℃ of the temperature, oxidation 4 hours, oxidizing process produces waste gas and absorbs with the 3M sodium hydroxide solution, vacuum cooled is to room temperature under the vacuum 0.08MPa, grind, promptly obtain novel imporous carbon absorbent material, be designated as A.
Embodiment 2:
Get sucrose, press mass ratio and add 98% sulfuric acid at 1: 2.5, stir, 160 ℃ of pre-oxidation are to bread-like, in 220 ℃, oxidation is 4.5 hours under the vacuum 0.07MPa, oxidizing process produces waste gas and absorbs with 4M sodium carbonate and 3M potassium hydroxide mixed solution, and vacuum cooled is ground to room temperature under the vacuum 0.08MPa, promptly obtain novel imporous carbon absorbent material, be designated as B.
Embodiment 3:
Get sucrose, press mass ratio and add 98% sulfuric acid at 1: 2.5, stir, 170 ℃ of pre-oxidation are to bread-like, in 230 ℃, oxidation is 4.5 hours under the vacuum 0.07MPa, oxidizing process produces the mixed solution absorption of waste gas with 4M NaOH and 6M sodium carbonate, and vacuum cooled is ground to room temperature under the vacuum 0.07MPa, promptly obtain novel imporous carbon absorbent material, be designated as C.
Embodiment 4:
Get sucrose, press mass ratio and add 98% sulfuric acid at 1: 3, stir, 160 ℃ of pre-oxidation are to bread-like, in 230 ℃, oxidation is 4.5 hours under the vacuum 0.06MPa, and oxidizing process produces waste gas 6M NaOH, and the mixed solution of 6M potassium hydroxide and 4M sodium carbonate absorbs, vacuum cooled is to room temperature under the vacuum 0.07MPa, grind, promptly obtain the novel imporous carbon absorbent material that gets, be designated as D.
Embodiment 5:
Get sucrose, press mass ratio and add 98% sulfuric acid at 1: 3, stir, 180 ℃ of pre-oxidation are to bread-like, in 230 ℃, oxidation is 5 hours under the vacuum 0.08MPa, oxidizing process produces the mixed solution absorption of waste gas with 3M potassium hydroxide and 6M sodium carbonate, and vacuum cooled is ground to room temperature under the vacuum 0.06MPa, promptly obtain novel imporous carbon absorbent material, be designated as E.
Embodiment 6:
Get sucrose, press mass ratio and add 98% sulfuric acid at 1: 4, stir, 180 ℃ of pre-oxidation are to bread-like, in 230 ℃, oxidation is 4.5 hours under the vacuum 0.06MPa, oxidizing process produces waste gas and absorbs with the 6M potassium hydroxide solution, and vacuum cooled is ground to room temperature under the vacuum 0.06MPa, promptly obtain novel imporous carbon absorbent material, be designated as F.
As shown in Figure 1, prepared novel carbon material adsorbing material particle diameter is 3~5 μ m, does not have obvious pore structure and exists; As shown in Figure 2, prepared imporous carbon absorbent material and other materials are compared the methylene blue adsorption effect, specific area of the present invention is 0.6m only
2/ g, but the adsorption capacity of methylene blue is better than commercially available active carbon; As shown in Figure 3, prepared imporous carbon absorbent material and other materials are compared Cr (VI) adsorption effect, the present invention reaches 60~70% of commercially available active carbon to the adsorption capacity of Cr (VI).Alternative active carbon is used for the adsorption treatment of heavy metal ions in wastewater and organic dyestuff.
Claims (3)
1. the preparation method of an imporous carbon absorbent material the steps include:
(1) gets sucrose, add 98% sulfuric acid charing, get the carbonaceous presoma by mass ratio 1: 2~4;
(2) carbonaceous presoma in above-mentioned (1) is heated to 150~180 ℃, pre-oxidation is to bread-like;
(3) with product in above-mentioned (2) in vacuum 0.06~0.08Mpa, under 220~230 ℃ of the temperature, continue oxidation 4~5 hours, the waste gas that is produced absorbs with alkali lye;
(4) vacuum cooled under vacuum 0.06~0.08MPa of product in above-mentioned (3) is ground to room temperature, promptly obtain imporous carbon absorbent material.
2. the preparation method of imporous carbon absorbent material according to claim 1 is characterized in that described charing method is 98% sulfuric acid charing, and carbonization temperature is a room temperature, sucrose and 98% sulfuric acid mass ratio 1: 2~4.
3. the preparation method of imporous carbon absorbent material according to claim 1 is characterized in that, it is 3~6M NaOH that oxidizing process absorbs waste gas alkali lye, perhaps potassium hydroxide, perhaps sodium carbonate liquor.
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CN102764631B (en) * | 2012-07-16 | 2014-07-09 | 中山大学 | Preparation method of porous semi-coke adsorbing material |
CN110975325A (en) * | 2019-10-23 | 2020-04-10 | 武汉科技大学 | Method for evaluating adsorption stability of heavy metal ion adsorbent based on solid-phase extraction |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20020187896A1 (en) * | 2001-04-30 | 2002-12-12 | Ryong Ryoo | Carbon molecular sieve and process for preparing the same |
CN1511784A (en) * | 2002-12-28 | 2004-07-14 | 谢仁智 | Process for preparing large and medium pore high performance active carbon |
CN1633334A (en) * | 2002-02-15 | 2005-06-29 | 亚乐克株式会社 | Adsorbent and process for producing adsorbent |
JP2006101829A (en) * | 2004-10-08 | 2006-04-20 | Mitsubishi Heavy Ind Ltd | System and method for producing syrup |
CN101121516A (en) * | 2007-08-07 | 2008-02-13 | 江西省绿野木业有限公司 | Multifunctional active carbon |
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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US20020187896A1 (en) * | 2001-04-30 | 2002-12-12 | Ryong Ryoo | Carbon molecular sieve and process for preparing the same |
CN1633334A (en) * | 2002-02-15 | 2005-06-29 | 亚乐克株式会社 | Adsorbent and process for producing adsorbent |
CN1511784A (en) * | 2002-12-28 | 2004-07-14 | 谢仁智 | Process for preparing large and medium pore high performance active carbon |
JP2006101829A (en) * | 2004-10-08 | 2006-04-20 | Mitsubishi Heavy Ind Ltd | System and method for producing syrup |
CN101121516A (en) * | 2007-08-07 | 2008-02-13 | 江西省绿野木业有限公司 | Multifunctional active carbon |
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JP特开2006101829A 2006.04.20 |
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