CN104477908A - Method for preparing activated carbon with chitosan used as raw material and obtainedactivated carbon - Google Patents
Method for preparing activated carbon with chitosan used as raw material and obtainedactivated carbon Download PDFInfo
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Abstract
The invention discloses a method for preparing activated carbon with chitosan used as a raw material. The chitosan is used as the raw material, and the specific processcomprises steps as follows: firstly, the chitosan is fully dispersed in an acetic acid aqueous solution with themass fraction of 1-10%, a chitosancolloidal solution with the mass fraction of 1-10% is prepared, hydro-thermal treatment is performed, a reaction is conducted at the temperature of 80-250 DEG C for 1-20 h, carbonizedchitosan is obtained through filtration, washing and drying treatment after the reaction, then thecarbonizedchitosan and sodium hydroxide powder are evenly mixed in the mass ratio ranging from 1:10 to 10:1 and placed into a vacuum tube type furnace to be calcined at the temperature of 100-1200 DEG C for 1-10 h, finally, a product is washed with deionized water and filtered until the pH ranges from 6 to 8, and an activated carbon material can be obtained through drying and grinding. According to the method,the activated carbon preparation process is simple, the production cost is low, and the obtained activated carbon is high in strength and large in specific surface area and has very high adsorption capacity.
Description
Technical field
The present invention relates to a kind of method preparing gac, is particularly the method that gac prepared by raw material with chitosan.
Background technology
Activated carbon pore structure is flourishing, and specific surface area is large, and high adsorption capacity, is widely used in the fields such as water treatment, desulfurization removing nitric, support of the catalyst, electrode materials, hydrogen storage material, luminescent material.Based on C element in gac, therefore all carbonaceous materials all may be used for Activated Carbon Production theoretically, and its raw material sources are quite extensive.Present life due to the expanded demand to gac, prepare that gac accounts for gac ultimate production with coal more than 67%, but coal belongs to Nonrenewable resources, in today that Mineral resources day is becoming tight, we must find other equivalent material and prepare gac.Make much progress in recent years, as utilized waste material composite reactive charcoal, common waste mainly contains fruit stone, stalk, bamboo, wood chip, mud etc.But these raw material supplies are limited, limit the industrial scale of gac, cause production cost high, Application Areas is less.Thus find activated carbon raw material cheap and easy to get, reducing production cost is prepare activated carbon process top priority.
Chitosan is a kind of natural alkaline kation polysaccharide, and abundance is cheap and easy to get.Chitosan is the deacetylated derivative of chitin, and under normal circumstances, the chitin of deacetylation more than 55% is called usually as chitosan.Chitin is a kind of a kind of natural high moleculer eompound extracted from crab shell, shrimp shell and fungal cell wall, and its annual biosynthesizing amount is only second to Mierocrystalline cellulose.
Summary of the invention
The object of this invention is to provide a kind of method preparing gac, this method take chitosan as raw material, solve the raw material problem of producing gac, adopt hydrothermal carbonization chitosan, the method that gac is prepared in activated process again shortens the time of preparing gac, the industrial scale expanding gac effectively, reduce production cost, energy efficient.
The present invention is that the method that gac prepared by raw material comprises the following steps with chitosan:
A. take chitosan as raw material, chitosan is well-dispersed in the acidic aqueous solution of massfraction 1 ~ 10%, make the chitosan gum liquid solution of massfraction 1 ~ 10%, and by clean for removal of bubbles in chitosan gum liquid solution;
B. hydrothermal carbonization, is transferred in tetrafluoroethylene autoclave by above-mentioned chitosan gum liquid solution, and baking oven reactor being placed in 80 ~ 250 DEG C carries out hydro-thermal reaction 1 ~ 20 hour.Reaction terminates rear taking-up reactor and naturally cools to room temperature, and precipitated product obtains carbonization chitosan through filtration, washing, drying treatment;
C. activate, by the carbonization chitosan obtained and activator in mass ratio 1:10 ~ 10:1 mix and put into vacuum tube furnace calcine 1 ~ 10 hour at 100 ~ 120 DEG C;
D. after product cooling, with distilled water wash, it is filtered to pH ≈ 6 ~ 8, dry, grinds the absorbent charcoal material that sieves to obtain;
Further, in technique scheme, described acidic aqueous solution is aqueous acetic acid or hydrochloric acid soln and other acidic aqueous solution that chitosan can be made to dissolve.
Further, in technique scheme, described washing fully can be washed to pH ≈ 6 ~ 8 with distilled water, also can combine fully washing to pH ≈ 6 ~ 8 by washing with alcohol or both.
Further, in technique scheme, described activator is selected from the arbitrary combination of more than any component of sodium hydroxide, potassium hydroxide, sodium carbonate and salt of wormwood or two kinds of components.
Further, in technique scheme, described reactivation process also can be carbonization chitosan powder, activator and distilled water in mass ratio 1:1:5 ~ 5:5:5 fully mix, soak 6 ~ 16 hours, after filtration, precipitation put into retort furnace and calcine 1 ~ 10 hour at 100 ~ 1200 DEG C.
Further, in technique scheme, described calcination process is for be warming up to 200 ~ 600 DEG C with 0.5 ~ 30 DEG C/min, be incubated 1 ~ 5 hour, then be warming up to 300 ~ 1200 DEG C with 0.5 ~ 30 DEG C/min, be incubated 1 ~ 5 hour, then be cooled to 200 ~ 700 DEG C, stop calcining.
Further, in technique scheme, it is cross the gac that 200 ~ 500 mesh sieve gained are preparation after grinding that described grinding is sieved.
The gac obtained by the above-mentioned method with chitosan being gac prepared by raw material, described activated carbon pore size 0.5nm ~ 100um, pore volume is 0.5 ~ 100cm
3/ g, specific surface area 1200 ~ 3000m
2/ g.
Beneficial effect of the present invention
1. use chitosan to prepare gac for raw material, solve raw material problem, expand the industrial scale of gac, reduce production cost, energy efficient, save the production time;
2. compared with prior art, the present invention is comparatively simple, and facility investment is few, and good product performance, intensity are high, is the new technology project of a low input, high production;
3. activated carbon pore size 0.5nm ~ 100um obtained by, pore volume is 0.5 ~ 50cm
3/ g, specific surface area 1200 ~ 3000m
2/ g;
4. activated carbon adsorptive capacity obtained by is strong, can reach 100 ~ 1000mg/g to the absorption of aqueous solution of methylene blue;
5. the method is by the reactor of the various volume of customization, and turnout is large;
6. the activator used in preparation process can recycling, greatly reduces costs.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph a of gac prepared by case study on implementation 1;
Fig. 2 is the stereoscan photograph b of gac prepared by case study on implementation 1;
Fig. 3 is the stereoscan photograph c of gac prepared by case study on implementation 1;
Fig. 4 is case study on implementation 2 chitosan activated carbon pore size distribution curve;
Fig. 5 is case study on implementation 2 chitosan gac N
2adsorption-desorption curve;
Fig. 6 is case study on implementation 2 chitosan gac pore volume curve.
Embodiment
Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.Test method described in following embodiment, if no special instructions, is ordinary method; Described reagent and material, if no special instructions, all can obtain from commercial channels, or can prepare in conventional manner.
Embodiment 1
A. take chitosan as raw material, chitosan is well-dispersed in the aqueous acetic acid of massfraction 2%, make the chitosan gum liquid solution of massfraction 2.5%, and by clean for removal of bubbles in chitosan gum liquid solution;
B. hydrothermal carbonization, is transferred in tetrafluoroethylene autoclave by above-mentioned chitosan gum liquid solution, and baking oven reactor being placed in 150 DEG C carries out hydro-thermal reaction 10 hours.Reaction terminates rear taking-up reactor and naturally cools to room temperature, precipitated product through filtering, distilled water fully washs to pH ≈ 7,70 DEG C of dryings and obtains carbonization chitosan in 8 hours;
C. activate, by the carbonization chitosan obtained and sodium hydroxide powder in mass ratio 1:10 mix and put into vacuum tube furnace and be warming up to 300 DEG C with 2 DEG C/min, constant temperature 2 hours, 500 DEG C are warming up to again with 2 DEG C/min, constant temperature 3 hours, is then cooled to 400 DEG C with 5 DEG C/min, stops calcining;
D. until product cooling after, with distilled water wash, it is filtered to pH ≈ 7,80 DEG C of dryings 6 hours, ground 300 mesh sieves absorbent charcoal material;
As shown in Figure 1, Figure 2, Figure 3 shows, be the stereoscan photograph of obtained absorbent charcoal material.
Embodiment 2
A. take chitosan as raw material, chitosan is well-dispersed in the aqueous acetic acid of massfraction 4%, make the chitosan gum liquid solution of massfraction 2.5%, and by clean for removal of bubbles in chitosan gum liquid solution;
B. hydrothermal carbonization, is transferred in tetrafluoroethylene autoclave by above-mentioned chitosan gum liquid solution, and baking oven reactor being placed in 160 DEG C carries out hydro-thermal reaction 12 hours.Reaction terminates rear taking-up reactor and naturally cools to room temperature, precipitated product through filtering, distilled water fully washs to pH ≈ 7 ,-50 DEG C of dryings and obtains carbonization chitosan in 8 hours;
C. activate, by the carbonization chitosan obtained and sodium hydroxide powder in mass ratio 1:1 mix and put into vacuum tube furnace and be warming up to 400 DEG C with 5 DEG C/min, constant temperature 1 hour, 800 DEG C are warming up to again with 4 DEG C/min, constant temperature 2 hours, is then cooled to 600 DEG C with 3 DEG C/min, stops calcining;
D. after product cooling, with distilled water wash, it is filtered to pH ≈ 7 ,-30 DEG C of dryings 10 hours, ground 300 mesh sieves absorbent charcoal material;
As shown in Figure 4, be the pore size distribution curve of the absorbent charcoal material obtained; Primary aperture is distributed in 3-5nm.
As seen from Figure 5, adsorption curve belongs to II type thermoisopleth in the classification of International Union of Pure and Applied Chemistry (IU-PAC) adsorption curve: S type thermoisopleth.The feature of this kind of absorption is: sorbent material under low pressure monolayer adsorption occurs, and pressure increases generation multilayer adsorption gradually, when pressure is quite high, because the gas of absorption has started to condense into liquid phase, so adsorptive capacity sharply rises again.Test result is specific surface area is 1294.66m
2/ g, monolayer adsorption amount is 297.4583cc/g.
As described in Figure 6, the pore volume 0.5-50cm of the absorbent charcoal material obtained
3/ g.
Embodiment 3
A. take chitosan as raw material, chitosan is well-dispersed in the aqueous acetic acid of massfraction 2%, make the chitosan gum liquid solution of massfraction 4%, and by clean for removal of bubbles in chitosan gum liquid solution;
B. hydrothermal carbonization, is transferred in tetrafluoroethylene autoclave by above-mentioned chitosan gum liquid solution, and baking oven reactor being placed in 180 DEG C carries out hydro-thermal reaction 24 hours.Reaction terminates rear taking-up reactor and naturally cools to room temperature, precipitated product through filtering, distilled water fully washs to pH ≈ 7 ,-20 DEG C of dryings and obtains carbonization chitosan in 6 hours;
C. activate, by the carbonization chitosan obtained and sodium hydroxide powder in mass ratio 1:2 mix and put into vacuum tube furnace and be warming up to 300 DEG C with 2 DEG C/min, constant temperature 2 hours, 500 DEG C are warming up to again with 2 DEG C/min, constant temperature 3 hours, is then cooled to 400 DEG C with 5 DEG C/min, stops calcining;
D. until product cooling after, with distilled water wash, it is filtered to pH ≈ 7,80 DEG C of dryings 10 hours, ground 300 mesh sieves absorbent charcoal material;
Embodiment 4
A. take chitosan as raw material, chitosan is well-dispersed in the aqueous acetic acid of massfraction 5%, make the chitosan gum liquid solution of massfraction 3%, and by clean for removal of bubbles in chitosan gum liquid solution;
B. hydrothermal carbonization, is transferred in tetrafluoroethylene autoclave by above-mentioned chitosan gum liquid solution, and baking oven reactor being placed in 150 DEG C carries out hydro-thermal reaction 18 hours.Reaction terminates rear taking-up reactor and naturally cools to room temperature, precipitated product through filtering, distilled water fully washs to pH ≈ 7,80 DEG C of dryings and obtains carbonization chitosan in 10 hours;
C. activate, by the carbonization chitosan obtained and sodium hydroxide powder in mass ratio 2:1 mix and put into vacuum tube furnace and be warming up to 200 DEG C with 3 DEG C/min, constant temperature 2 hours, 500 DEG C are warming up to again with 4 DEG C/min, constant temperature 3 hours, is then cooled to 400 DEG C with 5 DEG C/min, stops calcining;
D. after product cooling, with distilled water wash, it is filtered to pH ≈ 7 ,-30 DEG C of dryings 10 hours, ground 300 mesh sieves absorbent charcoal material;
Embodiment 5
A. take chitosan as raw material, chitosan is well-dispersed in the aqueous acetic acid of massfraction 2%, make the chitosan gum liquid solution of massfraction 2.5%, and by clean for removal of bubbles in chitosan gum liquid solution;
B. hydrothermal carbonization, is transferred in tetrafluoroethylene autoclave by above-mentioned chitosan gum liquid solution, and baking oven reactor being placed in 150 DEG C carries out hydro-thermal reaction 10 hours.Reaction terminates rear taking-up reactor and naturally cools to room temperature, precipitated product through filtering, distilled water fully washs to pH ≈ 7,70 DEG C of dryings and obtains carbonization chitosan in 8 hours;
C. activate, by above-mentioned carbonization chitosan and sodium hydroxide, distilled water in mass ratio 1:3:5 fully mix, soak 10 hours, after filtration, precipitation is put into vacuum tube furnace and be warming up to 200 DEG C with 3 DEG C/min, constant temperature 1 hour, then be warming up to 600 DEG C with 4 DEG C/min, constant temperature 2 hours, then be cooled to 200 DEG C with 5 DEG C/min, stop calcining;
D. until product cooling after, with distilled water wash, it is filtered to pH ≈ 7,80 DEG C of dryings 6 hours, ground 300 mesh sieves absorbent charcoal material;
Embodiment 6
A. take chitosan as raw material, chitosan is well-dispersed in the aqueous acetic acid of massfraction 4%, make the chitosan gum liquid solution of massfraction 3%, and by clean for removal of bubbles in chitosan gum liquid solution;
B. hydrothermal carbonization, is transferred in tetrafluoroethylene autoclave by above-mentioned chitosan gum liquid solution, and baking oven reactor being placed in 180 DEG C carries out hydro-thermal reaction 18 hours.Reaction terminates rear taking-up reactor and naturally cools to room temperature, precipitated product through filtering, distilled water fully washs to pH ≈ 7 ,-30 DEG C of dryings and obtains carbonization chitosan in 10 hours;
C. activate, by above-mentioned carbonization chitosan and sodium hydroxide, distilled water in mass ratio 1:1:5 fully mix, soak 12 hours, after filtration, precipitation is put into vacuum tube furnace and be warming up to 200 DEG C with 3 DEG C/min, constant temperature 1 hour, then be warming up to 600 DEG C with 4 DEG C/min, constant temperature 2 hours, then be cooled to 200 DEG C with 5 DEG C/min, stop calcining;
D. until product cooling after, with distilled water wash, it is filtered to pH ≈ 7,80 DEG C of dryings 6 hours, ground 300 mesh sieves absorbent charcoal material;
Embodiment 7
A. take chitosan as raw material, chitosan is well-dispersed in the aqueous acetic acid of massfraction 5%, make the chitosan gum liquid solution of massfraction 3%, and by clean for removal of bubbles in chitosan gum liquid solution;
B. hydrothermal carbonization, is transferred in tetrafluoroethylene autoclave by above-mentioned chitosan gum liquid solution, and baking oven reactor being placed in 180 DEG C carries out hydro-thermal reaction 18 hours.Reaction terminates rear taking-up reactor and naturally cools to room temperature, precipitated product through filtering, distilled water fully washs to pH ≈ 7,80 DEG C of dryings and obtains carbonization chitosan in 8 hours;
C. activate, by above-mentioned carbonization chitosan, sodium hydroxide and distilled water in mass ratio 1:2:5 fully mix, soak 10 hours, after filtration, precipitation is put into vacuum tube furnace and be warming up to 200 DEG C with 3 DEG C/min, constant temperature 1 hour, then be warming up to 600 DEG C with 4 DEG C/min, constant temperature 2 hours, then be cooled to 200 DEG C with 5 DEG C/min, stop calcining;
D. after product cooling, with distilled water wash, it is filtered to pH ≈ 7 ,-30 DEG C of dryings 10 hours, ground 300 mesh sieves absorbent charcoal material.
Embodiment 8
According to chitosan-gac prepared by embodiment 1-7.Adopt water Methylene Blue to be target affinity matter respectively, modulating pH in water is respectively 1,3,5,7,9,11, and room temperature condition records above-mentioned gac by Static Adsorption test all can reach 500-1000mg/g to the absorption of methylene blue.
Claims (8)
1. be the method that gac prepared by raw material with chitosan, it is characterized in that comprising the following steps:
A. take chitosan as raw material, chitosan is well-dispersed in the acidic aqueous solution of massfraction 1 ~ 10%, make the chitosan gum liquid solution of massfraction 1 ~ 10%, and by clean for removal of bubbles in chitosan gum liquid solution;
B. hydrothermal carbonization, the chitosan gum liquid solution obtained by step a is transferred in tetrafluoroethylene autoclave, baking oven reactor being placed in 80 ~ 250 DEG C carries out hydro-thermal reaction 1 ~ 20 hour, reaction terminates rear taking-up reactor and naturally cools to room temperature, and precipitated product obtains carbonization chitosan through filtration, washing, drying treatment;
C. activate, the carbonization chitosan obtained by step b and activator in mass ratio 1:10 ~ 10:1 mix and put into vacuum tube furnace calcine 1 ~ 10 hour at 100 ~ 1200 DEG C; Or the carbonization chitosan powder that step b obtained and activator, distilled water in mass ratio 1:1:5 ~ 1:5:5 fully mix, soak 6 ~ 16 hours, after filtration, precipitation to be put at vacuum tube furnace 100 ~ 1200 DEG C calcining 1 ~ 10 hour;
D. after product cooling, with distilled water wash, it is filtered to pH is 6 ~ 8, dry, grinds the absorbent charcoal material that sieves to obtain.
2. as claimed in claim 1 is the method that gac prepared by raw material with chitosan, it is characterized in that the acidic aqueous solution described in step a is aqueous acetic acid or hydrochloric acid soln.
3. as claimed in claim 1 or 2 is the method that gac prepared by raw material with chitosan, it is characterized in that: the washing described in step b is for being 6 ~ 8 by distilled water and/or washing with alcohol to pH.
4. as claimed in claim 1 or 2 is the method that gac prepared by raw material with chitosan, it is characterized in that the drying process described in step b, steps d is 30 ~ 100 DEG C, 6 ~ 10 hours or 0 ~-200 DEG C, 1 ~ 10 hour.
5. according to claim 1 and 2 is the method that gac prepared by raw material with chitosan, it is characterized in that: activator described in step c is selected from one or more in sodium hydroxide, potassium hydroxide, sodium carbonate, salt of wormwood.
6. according to claim 1 and 2 take chitosan as the method that gac prepared by raw material, it is characterized in that: the calcination process described in c is for be warming up to 200 ~ 600 DEG C with 0.5 ~ 30 DEG C/min, be incubated 1 ~ 5 hour, 300 ~ 1200 DEG C are warming up to again with 0.5 ~ 30 DEG C/min, be incubated 1 ~ 5 hour, then be cooled to 200 ~ 700 DEG C, stop calcining.
7. according to claim 1 and 2 is the method that gac prepared by raw material with chitosan, it is characterized in that the grinding described in steps d is sieved and is the gac of preparation for grinding rear mistake 200 ~ 500 mesh sieve gained.
8. take chitosan as the gac that the method that gac prepared by raw material obtains as described in claim 1 ~ 7 any one, and it is characterized in that: described activated carbon pore size 0.5nm ~ 100um, pore volume is 0.5 ~ 100cm
3/ g, specific surface area 1200 ~ 3000m
2/ g.
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