CN109607532A - A kind of preparation method of agar high specific surface area active charcoal - Google Patents
A kind of preparation method of agar high specific surface area active charcoal Download PDFInfo
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- CN109607532A CN109607532A CN201910076007.4A CN201910076007A CN109607532A CN 109607532 A CN109607532 A CN 109607532A CN 201910076007 A CN201910076007 A CN 201910076007A CN 109607532 A CN109607532 A CN 109607532A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
Abstract
The present invention discloses a kind of preparation method of agar high specific surface area active charcoal, it is related to technical field of active carbon, specifically includes the following steps: agar is add to deionized water stirring and dissolving by (1), 2.5-3.5 h, obtained agar based aquagel are stood after glutaraldehyde solution stirring is added；(2) porous agar is freeze-dried to obtain after agar based aquagel pre-freeze；(3) porous agar is cut into bulk, 500 DEG C is warming up in argon atmosphere, be carbonized 1-2h；(4) carbonized product is ground to partial size is 100-200 mesh; it is mixed with NaOH, KOH by weight 1:1:1-3; it is warming up to 600 DEG C under protection of argon gas; activation; after being naturally cooling to room temperature; activation crude product is successively washed till neutrality through HCl solution and deionized water, finally dries, obtains agar high specific surface area active charcoal.The active carbon large specific surface area, has excellent performance.
Description
Technical field
The present invention relates to technical field of active carbon, more particularly, to a kind of preparation side of agar high specific surface area active charcoal
Method.
Background technique
Carbon material is prepared as presoma because its is resourceful, cheap and easy to get, pollution-free and renewable etc. excellent using biomass
It puts and is paid close attention to by people.In recent years, people have carried out extensively prepares work with the plants such as shell, algae, fallen leaves presomas
The research work of property charcoal.
Chinese patent literature (CN107381573A) discloses a kind of absorbent charcoal material and preparation method thereof.Its technical solution
Are as follows: according to water: rich carbon organism: the mass ratio of potassium hydroxide is (2-1000): 1:(0.1-1.8), by the water, the rich carbon
Organism and potassium hydroxide mixing, stir 0.16-4h under the conditions of 40-1000 DEG C, obtain dark solution.By the black
Solution dries 2-4h under the conditions of 40-100 DEG C, obtains
Grey gel；The grey gel is protected into 0.5-12h under the conditions of 500-14000 DEG C in inert gas again, is washed, is done
It is dry, obtain absorbent charcoal material.The richness carbon organism is one of agar, glucose, sucrose, fructose, maltose.It is described lazy
Property gas is nitrogen or is hydrogen.The invention by rich carbon organism activate after direct carbonization, organism roasting when, surface or
Inside is easily broken, and reduces its specific surface area.
The preparation method that Chinese patent literature (106608625 B of CN) discloses a kind of mixed active charcoal, using Chinese hemp stalk and
Tree root prepares the active carbon of mixing material using one step activation method of phosphoric acid by activation, kneading, extruding etc. as raw material.It should
Patent is activated using Chinese hemp stalk, tree root, is mediated, extrusion process prepares active carbon, simple process, and specific surface area is small.
Summary of the invention
In view of this, in view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of agar base-height ratio surface areas to live
The preparation method of property charcoal, the active carbon large specific surface area of preparation are had excellent performance.
In order to achieve the above objectives, the invention adopts the following technical scheme:
A kind of preparation method of agar high specific surface area active charcoal, comprising the following steps:
(1) agar is added to stirring and dissolving in the deionized water of 9-11 times of weight, the glutaraldehyde that agar weight 2-4% is added is molten
Liquid, stirring 2-4min form mixed liquor, and mixed liquor is transferred to standing 2.5-3.5 h, obtained agar based aquagel in crystallising dish；
(2) agar based aquagel pre-freeze 6-10h at a temperature of -20 ~ -25 DEG C, it is freeze-dried to obtain porous agar；
(3) porous agar is cut into bulk, with 4-6 DEG C of min in argon atmosphere-1Speed be warming up to 500 DEG C, be carbonized 1-
2h；
(4) carbonized product is ground to partial size is 100-200 mesh, mixes with NaOH, KOH by weight 1:1:1-3, protects in argon gas
It is warming up to 600 DEG C under shield, activates 1.5 h, after being naturally cooling to room temperature, activates crude product successively through 1 mol L-1HCl solution
It is washed till neutrality with deionized water, it is finally dry at 50-70 DEG C, obtain agar high specific surface area active charcoal.
Further, the solution temperature of agar is 30-40 DEG C in the step (1), mixing time 2-3.5h.
Further, glutaraldehyde solution mass fraction is 20-30% in the step (1).
Further, the condenser temperature being freeze-dried in the step (2) is -50 DEG C, and drying pressure 100Pa adds
Hot plate temperature is 10 DEG C, drying time 18-24h.
Further, argon flow is 12-18mL min in the step (3)-1。
Further, heating rate is 5-7 DEG C of min in the step (4)-1, argon flow is 20 mL min-1。
The beneficial effects of the present invention are:
1, the present invention discloses a kind of agar high specific surface area active charcoal, and optimizes to its preparation process, the activity of preparation
Charcoal specific surface area is up to 3600-3900 m2·g-1, large specific surface area has excellent performance, and can be used for adsorbent material field.
2, during preparing active carbon, glutaraldehyde, i.e. agar and glutaraldehyde cross-linking are added in agar solution first,
The cross-linked gel structure stability of generation is higher, there is big gap in gel, and in roasting, its intensity is higher, it is not easy to and it is broken,
Specific surface area is bigger.
After agar based aquagel is freeze-dried, internal water sublimed forms cellular porous agar；Then exist
With 4-6 DEG C of min in argon atmosphere-1Speed be warming up to 500 DEG C, be carbonized；During slow heating, first in it
Remaining H, O can be escaped with vapor in portion, and in subsequent high temperature carbonisation, carbonaceous component is further formed gas evolution,
The slow heating mode can retain more carbon, improve the yield of product.
3, carbonized product is mixed with NaOH, KOH and is activated, wherein NaOH, KOH are gradually decomposed under high temperature action, most
End form can be inserted in the crystallite synusia of carbonaceous at potassium simple substance and sodium simple substance, deform so that carbonaceous material internal structure be issued,
To form new micropore, subsequent potassium simple substance and sodium simple substance are precipitated in vapour form, can greatly increase the specific surface area of product.
Specific embodiment
The present invention will be further described combined with specific embodiments below.
Embodiment 1
A kind of preparation method of agar high specific surface area active charcoal, comprising the following steps:
(1) agar is added to stirring and dissolving in the deionized water of 9 times of weight, solution temperature is 30 DEG C, mixing time 2h, so
The glutaraldehyde solution of agar weight 2% is added afterwards, wherein glutaraldehyde solution mass fraction is 20%, and stirring 2min forms mixed liquor,
Mixed liquor, which is transferred in crystallising dish, stands 2.5 h, obtained agar based aquagel；
(2) agar based aquagel pre-freeze 6h at a temperature of -20 DEG C, it is freeze-dried to obtain porous agar, wherein be freeze-dried
Condenser temperature is -50 DEG C, drying pressure 100Pa, and temperature of heating plate is 10 DEG C, drying time 18h；
(3) porous agar is cut into bulk, size is 3 × 3 × 3cm, with 4 DEG C of min in argon atmosphere-1Speed be warming up to
500 DEG C, wherein argon flow is 12mL min-1, be carbonized 1-2h；
(4) carbonized product is ground to partial size is 100 mesh, mixes with NaOH, KOH by weight 1:1:1, rises under protection of argon gas
Temperature is to 600 DEG C, and wherein heating rate is 5 DEG C of min-1, argon flow is 20 mL min-1, 1.5 h are activated at 600 DEG C, from
After being so cooled to room temperature, crude product is activated successively through 1 mol L-1HCl solution and deionized water be washed till neutrality, finally again will
Clean product is dry at 50 DEG C, obtains agar high specific surface area active charcoal.
Being detected its specific surface area is 3638 m2·g-1。
Embodiment 2
A kind of preparation method of agar high specific surface area active charcoal, comprising the following steps:
(1) agar is added to stirring and dissolving in the deionized water of 9.5 times of weight, solution temperature is 30 DEG C, and mixing time is
Then the glutaraldehyde solution of agar weight 3% is added in 2.5h, wherein glutaraldehyde solution mass fraction is 22%, and stirring 2min is formed
Mixed liquor, mixed liquor, which is transferred in crystallising dish, stands 2.5 h, obtained agar based aquagel；
(2) agar based aquagel pre-freeze 7h at a temperature of -20 DEG C, it is freeze-dried to obtain porous agar, wherein be freeze-dried
Condenser temperature is -50 DEG C, drying pressure 100Pa, and temperature of heating plate is 10 DEG C, drying time 19h；
(3) porous agar is cut into bulk, size is 3 × 3 × 3cm, with 4 DEG C of min in argon atmosphere-1Speed be warming up to
500 DEG C, wherein argon flow is 14mL min-1, be carbonized 1h；
(4) carbonized product is ground to partial size is 100 mesh, mixes with NaOH, KOH by weight 1:1:1, rises under protection of argon gas
Temperature is to 600 DEG C, and wherein heating rate is 5 DEG C of min-1, argon flow is 20 mL min-1, 1.5 h are activated at 600 DEG C, from
After being so cooled to room temperature, crude product is activated successively through 1 mol L-1HCl solution and deionized water be washed till neutrality, finally again will
Clean product is dry at 50 DEG C, obtains agar high specific surface area active charcoal.
Being detected its specific surface area is 3670m2·g-1。
Embodiment 3
A kind of preparation method of agar high specific surface area active charcoal, comprising the following steps:
(1) agar is added to stirring and dissolving in the deionized water of 10 times of weight, solution temperature is 35 DEG C, mixing time 3h,
Then the glutaraldehyde solution of agar weight 4% is added, wherein glutaraldehyde solution mass fraction is 25%, and stirring 3min forms mixing
Liquid, mixed liquor, which is transferred in crystallising dish, stands 3h, obtained agar based aquagel；
(2) agar based aquagel pre-freeze 8h at a temperature of -22 DEG C, it is freeze-dried to obtain porous agar, wherein be freeze-dried
Condenser temperature is -50 DEG C, drying pressure 100Pa, and temperature of heating plate is 10 DEG C, drying time 20h；
(3) porous agar is cut into bulk, size is 3 × 3 × 3cm, with 5 DEG C of min in argon atmosphere-1Speed be warming up to
500 DEG C, wherein argon flow is 15mL min-1, be carbonized 1.5h；
(4) carbonized product is ground to partial size is 150 mesh, mixes with NaOH, KOH by weight 1:1:2, rises under protection of argon gas
Temperature is to 600 DEG C, and wherein heating rate is 6 DEG C of min-1, argon flow is 20 mL min-1, 1.5 h are activated at 600 DEG C, from
After being so cooled to room temperature, crude product is activated successively through 1 mol L-1HCl solution and deionized water be washed till neutrality, finally again will
Clean product is dry at 60 DEG C, obtains agar high specific surface area active charcoal.
Being detected its specific surface area is 3872m2·g-1。
Embodiment 4
A kind of preparation method of agar high specific surface area active charcoal, comprising the following steps:
(1) agar is added to stirring and dissolving in the deionized water of 10.5 times of weight, solution temperature is 35 DEG C, and mixing time is
Then the glutaraldehyde solution of agar weight 2% is added in 3h, wherein glutaraldehyde solution mass fraction is 26%, and stirring 3min forms mixed
Liquid is closed, mixed liquor is transferred to standing 2.5-3.5 h, obtained agar based aquagel in crystallising dish；
(2) agar based aquagel pre-freeze 9h at a temperature of -22 DEG C, it is freeze-dried to obtain porous agar, wherein be freeze-dried
Condenser temperature is -50 DEG C, drying pressure 100Pa, and temperature of heating plate is 10 DEG C, drying time 22h；
(3) porous agar is cut into bulk, size is 3 × 3 × 3cm, with 5 DEG C of min in argon atmosphere-1Speed be warming up to
500 DEG C, wherein argon flow is 16mL min-1, be carbonized 1-2h；
(4) carbonized product is ground to partial size is 150 mesh, mixes with NaOH, KOH by weight 1:1:2, rises under protection of argon gas
Temperature is to 600 DEG C, and wherein heating rate is 6 DEG C of min-1, argon flow is 20 mL min-1, 1.5 h are activated at 600 DEG C, from
After being so cooled to room temperature, crude product is activated successively through 1 mol L-1HCl solution and deionized water be washed till neutrality, finally again will
Clean product is dry at 60 DEG C, obtains agar high specific surface area active charcoal.
Being detected its specific surface area is 3750 m2·g-1。
Embodiment 5
A kind of preparation method of agar high specific surface area active charcoal, comprising the following steps:
(1) agar is added to stirring and dissolving in the deionized water of 11 times of weight, solution temperature is 40 DEG C, and mixing time is
Then the glutaraldehyde solution of agar weight 3% is added in 3.5h, wherein glutaraldehyde solution mass fraction is 28%, and stirring 4min is formed
Mixed liquor, mixed liquor, which is transferred in crystallising dish, stands 3.5 h, obtained agar based aquagel；
(2) agar based aquagel pre-freeze 10h at a temperature of -25 DEG C, it is freeze-dried to obtain porous agar, wherein be freeze-dried
Condenser temperature is -50 DEG C, drying pressure 100Pa, and temperature of heating plate is 10 DEG C, drying time 23h；
(3) porous agar is cut into bulk, size is 3 × 3 × 3cm, with 6 DEG C of min in argon atmosphere-1Speed be warming up to
500 DEG C, wherein argon flow is 17mL min-1, be carbonized 2h；
(4) carbonized product is ground to partial size is 200 mesh, mixes with NaOH, KOH by weight 1:1:3, rises under protection of argon gas
Temperature is to 600 DEG C, and wherein heating rate is 7 DEG C of min-1, argon flow is 20 mL min-1, 1.5 h are activated at 600 DEG C, from
After being so cooled to room temperature, crude product is activated successively through 1 mol L-1HCl solution and deionized water be washed till neutrality, finally again will
Clean product is dry at 70 DEG C, obtains agar high specific surface area active charcoal.
Being detected its specific surface area is 3810 m2·g-1。
Embodiment 6
A kind of preparation method of agar high specific surface area active charcoal, comprising the following steps:
(1) agar is added to stirring and dissolving in the deionized water of 10 times of weight, solution temperature is 40 DEG C, and mixing time is
Then the glutaraldehyde solution of agar weight 4% is added in 2.5h, wherein glutaraldehyde solution mass fraction is 30%, and stirring 4min is formed
Mixed liquor, mixed liquor, which is transferred in crystallising dish, stands 3.5h, obtained agar based aquagel；
(2) agar based aquagel pre-freeze 10h at a temperature of -25 DEG C, it is freeze-dried to obtain porous agar, wherein be freeze-dried
Condenser temperature is -50 DEG C, drying pressure 100Pa, and temperature of heating plate is 10 DEG C, and drying time is for 24 hours；
(3) porous agar is cut into bulk, size is 3 × 3 × 3cm, with 6 DEG C of min in argon atmosphere-1Speed be warming up to
500 DEG C, wherein argon flow is 18mL min-1, be carbonized 2h；
(4) carbonized product is ground to partial size is 200 mesh, mixes with NaOH, KOH by weight 1:1:3, rises under protection of argon gas
Temperature is to 600 DEG C, and wherein heating rate is 7 DEG C of min-1, argon flow is 20 mL min-1, 1.5 h are activated at 600 DEG C, from
After being so cooled to room temperature, crude product is activated successively through 1 mol L-1HCl solution and deionized water be washed till neutrality, finally again will
Clean product is dry at 70 DEG C, obtains agar high specific surface area active charcoal.
Being detected its specific surface area is 3720m2·g-1。
Comparative example 1
Comparative example 1 is to remove the glutaraldehyde solution in the first step on the basis of embodiment 6, the specific steps are as follows:
A kind of preparation method of agar high specific surface area active charcoal, comprising the following steps:
(1) agar is added to stirring and dissolving in the deionized water of 10 times of weight, solution temperature is 40 DEG C, and mixing time is
2.5h is transferred in crystallising dish and stands 3.5h, obtained agar based aquagel；
(2) agar based aquagel pre-freeze 10h at a temperature of -25 DEG C, it is freeze-dried to obtain porous agar, wherein be freeze-dried
Condenser temperature is -50 DEG C, drying pressure 100Pa, and temperature of heating plate is 10 DEG C, and drying time is for 24 hours；
(3) porous agar is cut into bulk, size is 3 × 3 × 3cm, with 6 DEG C of min in argon atmosphere-1Speed be warming up to
500 DEG C, wherein argon flow is 18mL min-1, be carbonized 2h；
(4) carbonized product is ground to partial size is 200 mesh, mixes with NaOH, KOH by weight 1:1:3, rises under protection of argon gas
Temperature is to 600 DEG C, and wherein heating rate is 7 DEG C of min-1, argon flow is 20 mL min-1, 1.5 h are activated at 600 DEG C, from
After being so cooled to room temperature, crude product is activated successively through 1 mol L-1HCl solution and deionized water be washed till neutrality, finally again will
Clean product is dry at 70 DEG C, obtains agar high specific surface area active charcoal.
Being detected its specific surface area is 3415 m2·g-1。
Comparative example 2
Comparative example 2 is that step (4) activator is revised as KOH on the basis of embodiment 6, specific as follows:
A kind of preparation method of agar high specific surface area active charcoal, comprising the following steps:
(1) agar is added to stirring and dissolving in the deionized water of 10 times of weight, solution temperature is 40 DEG C, and mixing time is
Then the glutaraldehyde solution of agar weight 4% is added in 2.5h, wherein glutaraldehyde solution mass fraction is 30%, and stirring 4min is formed
Mixed liquor, mixed liquor, which is transferred in crystallising dish, stands 3.5h, obtained agar based aquagel；
(2) agar based aquagel pre-freeze 10h at a temperature of -25 DEG C, it is freeze-dried to obtain porous agar, wherein be freeze-dried
Condenser temperature is -50 DEG C, drying pressure 100Pa, and temperature of heating plate is 10 DEG C, and drying time is for 24 hours；
(3) porous agar is cut into bulk, size is 3 × 3 × 3cm, with 6 DEG C of min in argon atmosphere-1Speed be warming up to
500 DEG C, wherein argon flow is 18mL min-1, be carbonized 2h；
(4) carbonized product is ground to partial size is 200 mesh, mixes with KOH by weight 2:3, is warming up to 600 under protection of argon gas
DEG C, wherein heating rate is 7 DEG C of min-1, argon flow is 20 mL min-1, 1.5 h are activated at 600 DEG C, are naturally cooling to
After room temperature, crude product is activated successively through 1 mol L-1HCl solution and deionized water be washed till neutrality, production that finally again will be clean
Object is dry at 70 DEG C, obtains agar high specific surface area active charcoal.
It is 3590 m through specific surface area in detection comparative example 22·g-1。
The agar prepared by 1-6 of the embodiment of the present invention it can be seen from the testing result of embodiment 1-6 and comparative example 1-2
The specific surface area of high specific surface area active charcoal is 3600-3900 m2·g-1, comparative example 1 is on the basis of embodiment 6 by penta 2
Aldehyde removes, and without crosslinking, the specific surface area of the active carbon of preparation is smaller than embodiment 6, illustrates that glutaraldehyde and agar are crosslinked energy
The stability for enough increasing Cross-linked Agar, when agar is not with glutaraldehyde cross-linking, structure less stable, surface or internal appearance in roasting
Easily broken, specific surface area can accordingly reduce；And comparative example 2 is that activator is revised as KOH on the basis of embodiment 6, ratio
Surface area is also declined, and illustrates NaOH, KOH in activation, due to potassium simple substance and sodium simple substance partial size difference, the aperture of formation
It is not identical, there is synergistic effect.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, this field is common
Other modifications or equivalent replacement that technical staff makes technical solution of the present invention, without departing from technical solution of the present invention
Spirit and scope, be intended to be within the scope of the claims of the invention.
Claims (6)
1. a kind of preparation method of agar high specific surface area active charcoal, it is characterised in that: the following steps are included:
(1) agar is added to stirring and dissolving in the deionized water of 9-11 times of weight, the glutaraldehyde of agar weight 2-4% is added, stirs
It mixes 2-4min and forms mixed liquor, mixed liquor is transferred to standing 2.5-3.5 h, obtained agar based aquagel in crystallising dish；
(2) agar based aquagel pre-freeze 6-10h at a temperature of -20 ~ -25 DEG C, it is freeze-dried to obtain porous agar；
(3) porous agar is cut into bulk, with 4-6 DEG C of min in argon atmosphere-1Speed be warming up to 500 DEG C, be carbonized 1-2h；
(4) carbonized product is ground to partial size is 100-200 mesh, mixes with NaOH, KOH by weight 1:1:1-3, protects in argon gas
It is warming up to 600 DEG C under shield, activates 1.5 h, after being naturally cooling to room temperature, activates crude product successively through 1 mol L-1HCl solution
It is washed till neutrality with deionized water, it is finally dry at 50-70 DEG C, obtain agar high specific surface area active charcoal.
2. a kind of preparation method of agar high specific surface area active charcoal according to claim 1, it is characterised in that: described
The solution temperature of agar is 30-40 DEG C in step (1), mixing time 2-3.5h.
3. a kind of preparation method of agar high specific surface area active charcoal according to claim 1, it is characterised in that: described
Glutaraldehyde solution mass fraction is 20-30% in step (1).
4. a kind of preparation method of agar high specific surface area active charcoal according to claim 1, it is characterised in that: described
The condenser temperature being freeze-dried in step (2) is -50 DEG C, drying pressure 100Pa, and temperature of heating plate is 10 DEG C, when dry
Between be 18-24h.
5. a kind of preparation method of agar high specific surface area active charcoal according to claim 1, it is characterised in that: described
Argon flow is 12-18mL min in step (3)-1。
6. a kind of preparation method of agar high specific surface area active charcoal according to claim 1, it is characterised in that: described
Heating rate is 5-7 DEG C of min in step (4)-1, argon flow is 20 mL min-1。
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