CN109750392A - A kind of preparation method of asphalt activity carbon fiber cloth - Google Patents
A kind of preparation method of asphalt activity carbon fiber cloth Download PDFInfo
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- CN109750392A CN109750392A CN201711068447.2A CN201711068447A CN109750392A CN 109750392 A CN109750392 A CN 109750392A CN 201711068447 A CN201711068447 A CN 201711068447A CN 109750392 A CN109750392 A CN 109750392A
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Abstract
The invention discloses a kind of preparation methods of asphalt activity carbon fiber cloth, comprising the following steps: (1) impregnates pitch fibers cloth after washing with distilled water and dry after 3~5 hours in acetone；(2) pitch fibers are arranged in 200 DEG C of oxygen atmosphere, and cooling is taken out after being warming up to 400 DEG C of holdings 3~5 hours, cooling pitch fibers cloth is put into phosphate solution to impregnate 4~8 hours, takes out the drying of pitch fibers cloth after being kept for 2~4 hours to the temperature that phosphate solution is heated to 110~125 DEG C；(3) pitch fibers cloth is sent into the carbonizing apparatus for being connected with nitrogen, carbon dioxide is led to after being warming up to 750~850 DEG C, then stops logical carbon dioxide, water flowing steam is simultaneously warming up to 900~950 DEG C；(4) stop heating, be washed to neutrality after taking-up progress is air-cooled after natural cooling and dry.Activated carbon fiber cloth obtained by the present invention is based on mesoporous and is aided with micropore, large specific surface area and yield is higher.
Description
Technical field
The present invention relates to the preparation methods of activated carbon fiber cloth, more particularly, to a kind of system of asphalt activity carbon fiber cloth
Preparation Method.
Background technique
Activated carbon fiber cloth is activated carbon fiber series newcomer, using natural fiber cloth or Artificial Fibers cloth through pyrocarbon
Change, activate, has the characteristics that large specific surface area, pore are flourishing, absorbent properties are high, desorption rate is fast.It is widely used in molten
Agent recycling, air cleaning, water process, taste removal, deodorization, catalytic carrier, electrode material, health care, biochemical defence suit etc..It is presently commercially available
Asphalt activity carbon fiber cloth based on micropore, absorption aperture all concentrate on 2nm hereinafter, which limits it to divide greatly
The application of sub- adsorbing domain, the especially application in fields such as liquid phase adsorption, catalyst carrier, electronics, medical treatment.Therefore, micropore
Cooperate mesoporous activated carbon fiber cloth research and development be produced into order to activated carbon fiber cloth application extend important development direction it
One.
Summary of the invention
It is an object of the invention to overcome above-mentioned the deficiencies in the prior art, a kind of system of asphalt activity carbon fiber cloth is provided
Preparation Method, obtained activated carbon fiber cloth is based on mesoporous and is aided with micropore, large specific surface area and yield is higher.
In order to achieve the above objectives, the technical scheme is that a kind of preparation method of asphalt activity carbon fiber cloth, packet
Include following steps:
(1) selecting pitch fibers cloth is raw material, impregnates after distilled water cleans and is used for oil removing within 3~5 hours in acetone
And dehydration, room temperature then is carried out to pitch fibers cloth and is dried；
It (2) will be in the oxygen atmosphere for being 200 DEG C through step (1) treated pitch fibers are arranged in initial temperature, and with 5
DEG C/heating rate of min takes out natural cooling after being kept for 3~5 hours after rising to 400 DEG C, pitch fibers after cooling are laid
Enter in phosphate solution, in 5~10wt%, phosphate solution is ammonium phosphate, di(2-ethylhexyl)phosphate for the concentration control of the phosphate solution
Pitch fibers cloth is first put into phosphate solution 4~8 hours by one or both of hydrogen ammonium or diammonium hydrogen phosphate, then right
Phosphate solution is heated with the heating of 1 DEG C/min, and phosphate solution is finally controlled to the temperature holding 2 at 110~125 DEG C
It takes out pitch fibers cloth after~4 hours to be dried, drying temperature is controlled at 125~140 DEG C；
(3) it will be sent into carbonizing apparatus through step (2) treated pitch fibers cloth, and will be passed through nitrogen, in carbonizing apparatus with 5
DEG C/heating rate of min to 250~300 DEG C and keeps for 15 minutes, it to 500~600 DEG C and is protected with the heating rate of 8 DEG C/min
It holds 15 minutes, with the heating rate of 5 DEG C/min to carbon dioxide is passed through after 750~850 DEG C, is kept for 15~20 minutes, then stopped
Only lead to carbon dioxide, be passed through vapor and with the heating rate of 8 DEG C/min to 900~950 DEG C keep 20~30 minutes；
(4) stop heating, stop water flowing steam, continue to keep logical nitrogen, naturally cool to 200 DEG C or less taking-ups and carry out wind
It is washed to neutrality after cold and dries.
The pitch fibers cloth is the woven fabric made of pitch fibers, and the weight of pitch fibers cloth is 300-1000g/
m2。
The beneficial effects of the present invention are: obtained activated carbon fiber cloth is based on mesoporous and is aided with micropore, specific surface area
Big and yield is higher.
Specific embodiment
Below by embodiment, the technical solutions of the present invention will be further described.
Embodiment 1:
A kind of preparation method of asphalt activity carbon fiber cloth, comprising the following steps:
(1) selecting pitch fibers cloth is raw material, and the pitch fibers cloth is the woven fabric made of pitch fibers, and pitch is fine
The weight for tieing up cloth is 300g/m2, impregnated after distilled water cleans and be used for oil removing and dehydration within 3 hours in acetone, then to drip
Green fiber cloth carries out room temperature and dries；
It (2) will be in the oxygen atmosphere for being 200 DEG C through step (1) treated pitch fibers are arranged in initial temperature, and with 5
DEG C/heating rate of min takes out natural cooling after being kept for 3 hours after rising to 400 DEG C, pitch fibers cloth after cooling is put into phosphorus
In acid salt solution, the concentration of the phosphate solution is controlled in 5wt%, and phosphate solution is ammonium phosphate, first by pitch fibers cloth
It is put into ammonium phosphate 4 hours, then ammonium phosphate is heated with the heating of 1 DEG C/min, finally control ammonium phosphate at 110 DEG C
Temperature keep 2 hours after take out pitch fibers cloth dried, drying temperature control at 125 DEG C；
(3) it will be sent into carbonizing apparatus through step (2) treated pitch fibers cloth, and will be passed through nitrogen, in carbonizing apparatus with 5
DEG C/heating rate of min to 250 DEG C and keeps for 15 minutes, it to 500 DEG C and is kept for 15 minutes with the heating rate of 8 DEG C/min, with
The heating rate of 5 DEG C/min is kept for 15 minutes to carbon dioxide is passed through after 750 DEG C, then stops logical carbon dioxide, be passed through water steaming
Gas and with the heating rate of 8 DEG C/min to 900 DEG C keep 20 minutes；
(4) stop heating, stop water flowing steam, continue to keep logical nitrogen, naturally cool to 200 DEG C or less taking-ups and carry out wind
It is washed to neutrality after cold and dries.
The specific surface area of obtained asphalt activity carbon fiber cloth is 1870m2/ g, yield 29%, the aperture of mesoporous
For 38nm, the aperture of micropore is 0.9nm, and wherein mesoporous accounts for 72%, and remainder is micropore.
Embodiment 2:
A kind of preparation method of asphalt activity carbon fiber cloth, comprising the following steps:
(1) selecting pitch fibers cloth is raw material, and the pitch fibers cloth is the woven fabric made of pitch fibers, and pitch is fine
The weight for tieing up cloth is 450g/m2, impregnated after distilled water cleans and be used for oil removing and dehydration within 4 hours in acetone, then to drip
Green fiber cloth carries out room temperature and dries；
It (2) will be in the oxygen atmosphere for being 200 DEG C through step (1) treated pitch fibers are arranged in initial temperature, and with 5
DEG C/heating rate of min takes out natural cooling after being kept for 4 hours after rising to 400 DEG C, pitch fibers cloth after cooling is put into phosphorus
In acid salt solution, the concentration of the phosphate solution is controlled in 8wt%, and phosphate solution is ammonium dihydrogen phosphate, first by pitch fibre
Wei Bu is put into ammonium dihydrogen phosphate 6 hours, is then heated to ammonium dihydrogen phosphate with the heating of 1 DEG C/min, finally by phosphoric acid
Ammonium dihydrogen control, which takes out pitch fibers cloth after 120 DEG C of temperature is kept for 3 hours, is dried, and drying temperature is controlled at 135 DEG C；
(3) it will be sent into carbonizing apparatus through step (2) treated pitch fibers cloth, and will be passed through nitrogen, in carbonizing apparatus with 5
DEG C/heating rate of min to 270 DEG C and keeps for 15 minutes, it to 550 DEG C and is kept for 15 minutes with the heating rate of 8 DEG C/min, with
The heating rate of 5 DEG C/min is kept for 18 minutes to carbon dioxide is passed through after 800 DEG C, then stops logical carbon dioxide, be passed through water steaming
Gas and with the heating rate of 8 DEG C/min to 920 DEG C keep 25 minutes；
(4) stop heating, stop water flowing steam, continue to keep logical nitrogen, naturally cool to 200 DEG C or less taking-ups and carry out wind
It is washed to neutrality after cold and dries.
The specific surface area of obtained asphalt activity carbon fiber cloth is 2050m2/ g, yield 31%, the aperture of mesoporous
For 29nm, the aperture of micropore is 1nm, and wherein mesoporous accounts for 69%, and remainder is micropore.
Embodiment 3:
A kind of preparation method of asphalt activity carbon fiber cloth, comprising the following steps:
(1) selecting pitch fibers cloth is raw material, and the pitch fibers cloth is the woven fabric made of pitch fibers, and pitch is fine
The weight for tieing up cloth is 600g/m2, impregnated after distilled water cleans and be used for oil removing and dehydration within 5 hours in acetone, then to drip
Green fiber cloth carries out room temperature and dries；
It (2) will be in the oxygen atmosphere for being 200 DEG C through step (1) treated pitch fibers are arranged in initial temperature, and with 5
DEG C/heating rate of min takes out natural cooling after being kept for 5 hours after rising to 400 DEG C, pitch fibers cloth after cooling is put into phosphorus
In acid salt solution, the concentration of the phosphate solution is controlled in 10wt%, and phosphate solution is diammonium hydrogen phosphate, first by pitch fibre
Wei Bu is put into diammonium hydrogen phosphate 8 hours, is then heated to diammonium hydrogen phosphate with the heating of 1 DEG C/min, finally by phosphoric acid
The control of hydrogen diammonium, which takes out pitch fibers cloth after 125 DEG C of temperature is kept for 4 hours, is dried, and drying temperature is controlled at 140 DEG C；
(3) it will be sent into carbonizing apparatus through step (2) treated pitch fibers cloth, and will be passed through nitrogen, in carbonizing apparatus with 5
DEG C/heating rate of min to 300 DEG C and keeps for 15 minutes, it to 600 DEG C and is kept for 15 minutes with the heating rate of 8 DEG C/min, with
The heating rate of 5 DEG C/min is kept for 20 minutes to carbon dioxide is passed through after 850 DEG C, then stops logical carbon dioxide, be passed through water steaming
Gas and with the heating rate of 8 DEG C/min to 950 DEG C keep 30 minutes；
(4) stop heating, stop water flowing steam, continue to keep logical nitrogen, naturally cool to 200 DEG C or less taking-ups and carry out wind
It is washed to neutrality after cold and dries.
The specific surface area of obtained asphalt activity carbon fiber cloth is 2230m2/ g, yield 33%, the aperture of mesoporous
For 36nm, the aperture of micropore is 0.7nm, and wherein mesoporous accounts for 74%, and remainder is micropore.
Embodiment 4:
A kind of preparation method of asphalt activity carbon fiber cloth, comprising the following steps:
(1) selecting pitch fibers cloth is raw material, and the pitch fibers cloth is the woven fabric made of pitch fibers, and pitch is fine
The weight for tieing up cloth is 1000g/m2, it is impregnated after distilled water cleans and is used within 4.5 hours oil removing and dehydration in acetone, it is then right
Pitch fibers cloth carries out room temperature and dries；
It (2) will be in the oxygen atmosphere for being 200 DEG C through step (1) treated pitch fibers are arranged in initial temperature, and with 5
DEG C/heating rate of min takes out natural cooling after being kept for 3.5 hours after rising to 400 DEG C, pitch fibers cloth after cooling is put into
In phosphate solution, for the control of the concentration of the phosphate solution in 9wt%, phosphate solution is ammonium phosphate and ammonium dihydrogen phosphate,
First pitch fibers cloth is put into phosphate solution 4 hours, then phosphate solution is heated with the heating of 1 DEG C/min,
Phosphate solution is finally controlled the taking-up pitch fibers cloth behind temperature holding 2 hours of 110 DEG C to dry, drying temperature control
System is at 125 DEG C；
(3) it will be sent into carbonizing apparatus through step (2) treated pitch fibers cloth, and will be passed through nitrogen, in carbonizing apparatus with 5
DEG C/heating rate of min to 250 DEG C and keeps for 15 minutes, it to 500 DEG C and is kept for 15 minutes with the heating rate of 8 DEG C/min, with
The heating rate of 5 DEG C/min is kept for 15 minutes to carbon dioxide is passed through after 750 DEG C, then stops logical carbon dioxide, be passed through water steaming
Gas and with the heating rate of 8 DEG C/min to 900 DEG C keep 20 minutes；
(4) stop heating, stop water flowing steam, continue to keep logical nitrogen, naturally cool to 200 DEG C or less taking-ups and carry out wind
It is washed to neutrality after cold and dries.
The specific surface area of obtained asphalt activity carbon fiber cloth is 1760m2/ g, yield 41%, the aperture of mesoporous
For 20nm, the aperture of micropore is 0.8nm, and wherein mesoporous accounts for 64%, and remainder is micropore.
Embodiment 5:
A kind of preparation method of asphalt activity carbon fiber cloth, comprising the following steps:
(1) selecting pitch fibers cloth is raw material, and the pitch fibers cloth is the woven fabric made of pitch fibers, and pitch is fine
The weight for tieing up cloth is 800g/m2, impregnated after distilled water cleans and be used for oil removing and dehydration within 4 hours in acetone, then to drip
Green fiber cloth carries out room temperature and dries；
It (2) will be in the oxygen atmosphere for being 200 DEG C through step (1) treated pitch fibers are arranged in initial temperature, and with 5
DEG C/heating rate of min takes out natural cooling after being kept for 4.5 hours after rising to 400 DEG C, pitch fibers cloth after cooling is put into
In phosphate solution, in 7.5wt%, phosphate solution is ammonium phosphate and phosphoric acid hydrogen two for the concentration control of the phosphate solution
Pitch fibers cloth is first put into phosphate solution 6 hours, is then added to phosphate solution with the heating of 1 DEG C/min by ammonium
Phosphate solution is finally controlled the taking-up pitch fibers cloth behind temperature holding 3 hours of 120 DEG C and dried by heat, drying temperature
Degree control is at 135 DEG C；
(3) it will be sent into carbonizing apparatus through step (2) treated pitch fibers cloth, and will be passed through nitrogen, in carbonizing apparatus with 5
DEG C/heating rate of min to 280 DEG C and keeps for 15 minutes, it to 270 DEG C and is kept for 15 minutes with the heating rate of 8 DEG C/min, with
The heating rate of 5 DEG C/min is kept for 19 minutes to carbon dioxide is passed through after 820 DEG C, then stops logical carbon dioxide, be passed through water steaming
Gas and with the heating rate of 8 DEG C/min to 930 DEG C keep 27 minutes；
(4) stop heating, stop water flowing steam, continue to keep logical nitrogen, naturally cool to 200 DEG C or less taking-ups and carry out wind
It is washed to neutrality after cold and dries.
The specific surface area of obtained asphalt activity carbon fiber cloth is 2310m2/ g, yield 39%, the aperture of mesoporous
For 19nm, the aperture of micropore is 1.2nm, and wherein mesoporous accounts for 66%, and remainder is micropore.
Embodiment 6:
A kind of preparation method of asphalt activity carbon fiber cloth, comprising the following steps:
(1) selecting pitch fibers cloth is raw material, and the pitch fibers cloth is the woven fabric made of pitch fibers, and pitch is fine
The weight for tieing up cloth is 700g/m2, impregnated after distilled water cleans and be used for oil removing and dehydration within 5 hours in acetone, then to drip
Green fiber cloth carries out room temperature and dries；
It (2) will be in the oxygen atmosphere for being 200 DEG C through step (1) treated pitch fibers are arranged in initial temperature, and with 5
DEG C/heating rate of min takes out natural cooling after being kept for 5 hours after rising to 400 DEG C, pitch fibers cloth after cooling is put into phosphorus
In acid salt solution, in 10wt%, phosphate solution is ammonium dihydrogen phosphate and phosphoric acid hydrogen two for the concentration control of the phosphate solution
Pitch fibers cloth is first put into phosphate solution 8 hours, is then added to phosphate solution with the heating of 1 DEG C/min by ammonium
Phosphate solution is finally controlled the taking-up pitch fibers cloth behind temperature holding 4 hours of 125 DEG C and dried by heat, drying temperature
Degree control is at 140 DEG C；
(3) it will be sent into carbonizing apparatus through step (2) treated pitch fibers cloth, and will be passed through nitrogen, in carbonizing apparatus with 5
DEG C/heating rate of min to 300 DEG C and keeps for 15 minutes, it to 600 DEG C and is kept for 15 minutes with the heating rate of 8 DEG C/min, with
The heating rate of 5 DEG C/min is kept for 20 minutes to carbon dioxide is passed through after 850 DEG C, then stops logical carbon dioxide, be passed through water steaming
Gas and with the heating rate of 8 DEG C/min to 950 DEG C keep 30 minutes；
(4) stop heating, stop water flowing steam, continue to keep logical nitrogen, naturally cool to 200 DEG C or less taking-ups and carry out wind
It is washed to neutrality after cold and dries.
The specific surface area of obtained asphalt activity carbon fiber cloth is 2450m2/ g, yield 34%, the aperture of mesoporous
For 16nm, the aperture of micropore is 1.0nm, and wherein mesoporous accounts for 78%, and remainder is micropore.
The foregoing is merely the preferable specific embodiments of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.
Claims (2)
1. a kind of preparation method of asphalt activity carbon fiber cloth, it is characterised in that: the following steps are included:
(1) selecting pitch fibers cloth is raw material, impregnates after distilled water cleans and is used within 3~5 hours oil removing in acetone and takes off
Then water carries out room temperature to pitch fibers cloth and dries；
(2) will in the oxygen atmosphere for being 200 DEG C through step (1) treated pitch fibers are arranged in initial temperature, and with 5 DEG C/
The heating rate of min takes out natural cooling after being kept for 3~5 hours after rising to 400 DEG C, and pitch fibers cloth after cooling is put into phosphorus
In acid salt solution, in 5~10wt%, phosphate solution is ammonium phosphate, ammonium dihydrogen phosphate for the concentration control of the phosphate solution
Or one or both of diammonium hydrogen phosphate, first pitch fibers cloth is put into phosphate solution 4~8 hours, then to phosphoric acid
Salting liquid is heated with the heating of 1 DEG C/min, and phosphate solution is finally controlled to the temperature holding 2~4 at 110~125 DEG C
It takes out pitch fibers cloth after hour to be dried, drying temperature is controlled at 125~140 DEG C；
(3) carbonizing apparatus will be sent into through step (2) treated pitch fibers cloth, nitrogen is passed through in carbonizing apparatus, with 5 DEG C/
The heating rate of min to 250~300 DEG C and keep 15 minutes, with the heating rate of 8 DEG C/min to 500~600 DEG C and keep 15
Minute, with the heating rate of 5 DEG C/min to carbon dioxide is passed through after 750~850 DEG C, is kept for 15~20 minutes, then stopped logical
Carbon dioxide, be passed through vapor and with the heating rate of 8 DEG C/min to 900~950 DEG C keep 20~30 minutes；
(4) stop heating, stop water flowing steam, continue to keep logical nitrogen, naturally cool to 200 DEG C or less taking-ups progress it is air-cooled after
It is washed to neutrality and dries.
2. a kind of preparation method of asphalt activity carbon fiber cloth as described in claim 1, it is characterised in that: the pitch fibers
Cloth is the woven fabric made of pitch fibers, and the weight of pitch fibers cloth is 300-1000g/m2。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711068447.2A CN109750392A (en) | 2017-11-02 | 2017-11-02 | A kind of preparation method of asphalt activity carbon fiber cloth |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711068447.2A CN109750392A (en) | 2017-11-02 | 2017-11-02 | A kind of preparation method of asphalt activity carbon fiber cloth |
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| CN109750392A true CN109750392A (en) | 2019-05-14 |
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|---|---|---|---|
| CN201711068447.2A Pending CN109750392A (en) | 2017-11-02 | 2017-11-02 | A kind of preparation method of asphalt activity carbon fiber cloth |
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- 2017-11-02 CN CN201711068447.2A patent/CN109750392A/en active Pending
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Application publication date: 20190514 |