CN101816930B - Method for preparing carbon wrapped micro-silica powder adsorption material - Google Patents
Method for preparing carbon wrapped micro-silica powder adsorption material Download PDFInfo
- Publication number
- CN101816930B CN101816930B CN2009101175040A CN200910117504A CN101816930B CN 101816930 B CN101816930 B CN 101816930B CN 2009101175040 A CN2009101175040 A CN 2009101175040A CN 200910117504 A CN200910117504 A CN 200910117504A CN 101816930 B CN101816930 B CN 101816930B
- Authority
- CN
- China
- Prior art keywords
- sucrose
- silica powder
- adsorption material
- micro
- silica
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a method for preparing a carbon wrapped micro-silica powder adsorption material, which comprises the following steps of: firstly, taking sucrose, adding water into the sucrose to dissolve partial sucrose, and mixing the sucrose solution and 98 percent ammonium sulfate in a mass ratio of 1: 2-4 to obtain a carbon precursor; secondly, quickly mixing the carbon precursor and micro-silica powder of which the silicon dioxide content is over 65 percent in a mass ratio of the sucrose to the micro-silica powder of 1: 0.2 to 2, and stirring the mixture to form paste; thirdly, heating the paste to between 150 and 180 DEG C, and pre-oxidizing the paste to form a bread-like product; fourthly, continuously oxidizing the product for 4 to 5 hours at the temperature of between 220and 230 DEG under vacuum of 0.06 to 0.08MPa, and absorbing the produced waste gas by using alkali liquor; and finally, cooling the product to room temperature under the vacuum of 0.06 to 0.08MPa, and grinding the product to obtain the carbon wrapped micro-silica powder adsorption material.
Description
Technical field
The present invention relates to a kind of preparation method of sorbing material.
Background technology
SILICA FUME is a kind of Powdered discarded object that industry such as ferrosilicon produces, average grain diameter 30～300nm, and main component is a silica, impurity is main with metal oxide and indefinite form charcoal.Dioxide-containing silica is very big according to the different difference of recovery technology.Dioxide-containing silica is higher than 85% SILICA FUME, general as cheap construction material alloy use, for the low content SILICA FUME, then need make it reach instructions for use through technologies such as calcination, acidleach.China's SILICA FUME output is huge, but owing to reasons such as equipment and technology, most of SILICA FUME dioxide-containing silicas do not reach instructions for use, and purifying needs to consume mass energy and acid solution, and the very difficult recycling of acid solution, and environment is caused secondary pollution.
To the development and use of the profound high added value of SILICA FUME resource, particularly, just at the early-stage at present to the utilization of low content SILICA FUME.Chinese patent CN101293656A and Chinese patent CN101293754A utilize SILICA FUME to prepare compound white carbon and titanium dioxide composite material respectively; Not only expanded the scope of application of SILICA FUME resource; Improve its use value, also promoted the enthusiasm that manufacturing enterprise reclaims the SILICA FUME resource.The weak point of these patents is to need SILICA FUME acidleach removal of impurities is handled, and consumes a large amount of acid solutions and can't reclaim.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of carbon wrapped micro-silica powder adsorption material.
The present invention is a kind of preparation method of carbon wrapped micro-silica powder adsorption material, the steps include:
(1) gets sucrose, add water and make it to be partly dissolved, mix by mass ratio 1: 2～4, get the carbonaceous presoma with 98% sulfuric acid;
(2) with carbonaceous presoma in above-mentioned (1) and dioxide-containing silica greater than 65% SILICA FUME by quality than sucrose: mix rapidly SILICA FUME=1: 0.2～2, is stirred to pasty state;
(3) pastel in above-mentioned (2) is heated to 150～180 ℃, pre-oxidation is to bread-like;
(4) with product in above-mentioned (3) 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;
(5) product in above-mentioned (4) is cooled to room temperature under vacuum 0.06～0.08MPa, grinds, promptly obtain carbon wrapped micro-silica powder adsorption material.
The present invention has following advantage:
1, 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.
2, be raw material with dioxide-containing silica greater than 65% SILICA FUME, SILICA FUME does not need pre-treatment directly to use.
3, oxidizing process is utilized the oxidisability of the concentrated sulfuric acid self, need not oxidant applying; Oxidizing process is carried out in a vacuum, helps protecting the charcoal particle of SILICA FUME surface parcel, 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 wrapped micro-silica powder adsorption material reaches 70～80% of commercially available active carbon to the adsorption capacity of Cr (VI) and methylene blue, and the cheaper alternative that can be used as 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 the preceding SILICA FUME of charcoal parcel; Fig. 2 is the SEM figure of charcoal parcel back (b) SILICA FUME; Fig. 3 is prepared carbon wrapped micro-silica powder adsorption material and the other materials adsorption effect comparison diagram to Cr (VI), and Fig. 4 is prepared carbon wrapped micro-silica powder adsorption material and the other materials adsorption effect comparison diagram to methylene blue.
The specific embodiment
Embodiment 1:
Get sucrose, add water and make it to be partly dissolved, with 98% sulfuric acid by quality than sucrose: 98% sulfuric acid=mix at 1: 2; Again rapidly with the SILICA FUME of dioxide-containing silica 65.7% by sucrose: the mass ratio of SILICA FUME=1: 0.2 mixes, and is stirred to pasty state, and 150 ℃ of pre-oxidation are to bread-like; In vacuum 0.06Mpa, under 220 ℃ of the temperature, oxidation 4 hours; Oxidizing process produces waste gas and absorbs with the 3M sodium hydroxide solution, is cooled to room temperature under the vacuum 0.06MPa, grinds; Promptly obtain carbon wrapped micro-silica powder adsorption material, be designated as A.
Embodiment 2:
Get sucrose, add water and make it to be partly dissolved, with 98% sulfuric acid by quality than sucrose: 98% sulfuric acid=mix at 1: 2.5; Again rapidly with the SILICA FUME of dioxide-containing silica 76.5% by sucrose: the mass ratio of SILICA FUME=1: 0.5 mixes, and is stirred to pasty state, and 160 ℃ of pre-oxidation are to bread-like; In vacuum 0.07MPa, under 220 ℃ of the temperature, oxidation 4.5 hours; Oxidizing process produces waste gas and absorbs with the 4M potassium hydroxide solution, is cooled to room temperature under the vacuum 0.06MPa, grinds; Promptly obtain carbon wrapped micro-silica powder adsorption material, be designated as B.
Embodiment 3:
Get sucrose, add water and make it to be partly dissolved, with 98% sulfuric acid by quality than sucrose: 98% sulfuric acid=mix at 1: 2.5; Again rapidly with the SILICA FUME of dioxide-containing silica 82.1% by sucrose: the mass ratio of SILICA FUME=1: 1 mixes, and is stirred to pasty state, and 170 ℃ of pre-oxidation are to bread-like; In vacuum 0.08MPa, under 230 ℃ of the temperature, oxidation 4.5 hours; Oxidizing process produces the mixed solution absorption of waste gas with 3M NaOH and 3M potash, is cooled to room temperature under the vacuum 0.06MPa, grinds; Promptly obtain carbon wrapped micro-silica powder adsorption material, be designated as C.
Embodiment 4:
Get sucrose, add water and make it to be partly dissolved, with 98% sulfuric acid by quality than sucrose: 98% sulfuric acid=mix at 1: 3; Again rapidly with the SILICA FUME of dioxide-containing silica 85.4% by sucrose: the mass ratio of SILICA FUME=1: 1 mixes, and is stirred to pasty state, and 160 ℃ of pre-oxidation are to bread-like; In vacuum 0.06MPa, under 230 ℃ of the temperature, oxidation 4.5 hours; Oxidizing process produces waste gas and absorbs with the 5M sodium carbonate liquor, is cooled to room temperature under the vacuum 0.07MPa, grinds; Promptly obtain carbon wrapped micro-silica powder adsorption material, be designated as D.
Embodiment 5:
Get sucrose, add water and make it to be partly dissolved, with 98% sulfuric acid by quality than sucrose: 98% sulfuric acid=mix at 1: 3; Again rapidly with the SILICA FUME of dioxide-containing silica 91.3% by sucrose: the mass ratio of SILICA FUME=1: 1.5 mixes, and is stirred to pasty state, and 180 ℃ of preliminary treatment are to bread-like; In vacuum 0.07MPa, under 230 ℃ of the temperature, oxidation 5 hours; Oxidizing process produces waste gas and absorbs with the 5M potassium hydroxide solution, is cooled to room temperature under the vacuum 0.08MPa, grinds; Promptly obtain carbon wrapped micro-silica powder adsorption material, be note E.
Embodiment:
Get sucrose, add water and make it to be partly dissolved, with 98% sulfuric acid by quality than sucrose: 98% sulfuric acid=mix at 1: 4; Again rapidly with the SILICA FUME of dioxide-containing silica 93.0% by sucrose: the mass ratio of SILICA FUME=1: 2 mixes, and is stirred to pasty state, and 180 ℃ of pre-oxidation are to bread-like; In vacuum 0.08MPa, under 230 ℃ of the temperature, oxidation 5 hours; Oxidizing process produces waste gas and absorbs with the 6M sodium hydroxide solution, is cooled to room temperature under the vacuum 0.08MPa, grinds; Promptly obtain novel carbon wrapped micro-silica powder adsorption material, be designated as F.
Like Fig. 1, shown in Figure 2,, confirm that prepared carbon wrapped micro-silica powder adsorption material specific area reaches 51m2/g through the SEM figure of SILICA FUME before the contrast charcoal parcel and the SEM figure of charcoal parcel back SILICA FUME; Like Fig. 3, shown in Figure 4, carbon wrapped micro-silica powder adsorption material reaches 70～80% of commercially available active carbon to the adsorption capacity of Cr (VI) and methylene blue, and alternative active carbon is used for the adsorption treatment of heavy metal ions in wastewater and organic dyestuff.
Claims (2)
1. the preparation method of a carbon wrapped micro-silica powder adsorption material the steps include:
(1) gets sucrose, add water and make it to be partly dissolved, mix by mass ratio 1: 2～4, get the carbonaceous presoma with 98% sulfuric acid;
(2) with carbonaceous presoma in above-mentioned (1) and dioxide-containing silica greater than 65% SILICA FUME by quality than sucrose: mix rapidly SILICA FUME=1: 0.2～2, is stirred to pasty state;
(3) pastel in above-mentioned (2) is heated to 150～180 ℃, pre-oxidation is to bread-like;
(4) with product in above-mentioned (3) 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;
(5) product in above-mentioned (4) is cooled to room temperature under vacuum 0.06～0.08MPa, grinds, promptly obtain carbon wrapped micro-silica powder adsorption material.
2. the preparation method of carbon wrapped micro-silica powder adsorption material according to claim 1 is characterized in that, it is 3～6M NaOH that the oxidizing process absorbing waste gas is used alkali lye, perhaps potassium hydroxide solution, perhaps sodium carbonate liquor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101175040A CN101816930B (en) | 2009-10-10 | 2009-10-10 | Method for preparing carbon wrapped micro-silica powder adsorption material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101175040A CN101816930B (en) | 2009-10-10 | 2009-10-10 | Method for preparing carbon wrapped micro-silica powder adsorption material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101816930A CN101816930A (en) | 2010-09-01 |
| CN101816930B true CN101816930B (en) | 2012-05-30 |
Family
ID=42652293
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009101175040A Expired - Fee Related CN101816930B (en) | 2009-10-10 | 2009-10-10 | Method for preparing carbon wrapped micro-silica powder adsorption material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101816930B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106423041A (en) * | 2016-11-09 | 2017-02-22 | 山东科技大学 | Micro-silicon powder adsorption material and preparation method and application thereof |
| CN107601516B (en) * | 2017-09-26 | 2019-09-06 | 湖北工程学院 | A kind of carbon coating boron doping silica nano material and preparation method thereof |
-
2009
- 2009-10-10 CN CN2009101175040A patent/CN101816930B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN101816930A (en) | 2010-09-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108054366B (en) | Lithium ion battery cathode material and preparation method thereof | |
| CN103427069B (en) | A kind of composite cathode material for lithium ion cell and preparation thereof | |
| WO2015106720A1 (en) | Method for producing super activated charcoal from biomass power plant ash | |
| CN105870422A (en) | C@SiOx material, preparation method thereof and application of C@SiOx material taken as negative electrode material of lithium ion battery | |
| CN101710632A (en) | Method for recovering and restoring anode material graphite of waste lithium ion battery | |
| CN102544629A (en) | Method for regenerating waste and old graphite anode materials | |
| CN100377395C (en) | Nano composite lithium ion cell cathode material and its preparing method | |
| CN108155343A (en) | Lithium ion battery pulping process | |
| CN105140471A (en) | MoS2/C lithium-ion battery anode composite material and preparation method thereof | |
| CN115490223B (en) | Preparation method of hard carbon negative electrode material based on waste phenolic resin | |
| CN103199319B (en) | Method for recycling lithium cobalt oxide from waste positive electrode of lithium cobalt oxide battery | |
| CN108622887B (en) | Method for preparing graphene through microwave puffing | |
| CN101816930B (en) | Method for preparing carbon wrapped micro-silica powder adsorption material | |
| CN104843800A (en) | Solvothermal preparation method for carbon-coated ferriferrous oxide negative electrode material | |
| CN115000359B (en) | Method for preparing lithium battery negative electrode material by utilizing graphite tailings | |
| CN108054396A (en) | A kind of nitrogen-doped graphene/cobalt protoxide composite material and preparation method thereof | |
| CN103326022A (en) | Method for preparing lithium ferrous silicate positive pole material from ilmenite | |
| CN102642844A (en) | Lithium chloride molten salt method for preparing lanthanum silicate electrolyte material powder with oxidapatite structure | |
| CN103236543B (en) | Method for preparing lithium ferrous silicate anode material | |
| CN115548322A (en) | Preparation method and application of modified microcrystalline graphite secondary particle negative electrode material | |
| WO2019127031A1 (en) | Energy composite material for lithium battery and preparation method therefor | |
| CN113104845B (en) | Method for preparing porous artificial graphite cathode material by using electrode joint powder as raw material | |
| CN104934583B (en) | Preparation method of elemental silicon-graphene nanoribbon composite material | |
| CN114604850A (en) | Preparation method and application of porous microsphere carbon negative electrode material | |
| CN107146887A (en) | Carbon nanometer three-dimensional structure composite for negative electrode of lithium ion battery and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120530 Termination date: 20131010 |