CN106040172A - Preparation method of viscose-based activated carbon fiber cloth - Google Patents
Preparation method of viscose-based activated carbon fiber cloth Download PDFInfo
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- CN106040172A CN106040172A CN201610428234.5A CN201610428234A CN106040172A CN 106040172 A CN106040172 A CN 106040172A CN 201610428234 A CN201610428234 A CN 201610428234A CN 106040172 A CN106040172 A CN 106040172A
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- viscose rayon
- cloth
- viscose
- impregnation liquid
- fiber cloth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
Abstract
The invention discloses a preparation method of viscose-based activated carbon fiber cloth. The preparation method comprises the following steps: (1) after cleaning viscose fiber cloth with distilled water, soaking in acetone for 3-5 hours, and then drying at normal temperature; (2) soaking the viscose fiber cloth in steeping fluid for 5-10 hours, then heating the steeping fluid at heating speed of 1 DEG C per minute, finally controlling the steeping fluid at the temperature of 80-95 DEG C for 5-8 hours, then taking out the viscose fiber cloth and drying; (3) feeding the viscose fiber cloth into carbonization equipment, feeding nitrogen into the carbonization equipment, after heating to the temperature of 750-850 DEG C, then feeding carbon dioxide, after maintaining for 15-20 minutes, feeding mixed gas of the carbon dioxide and water valor, then heating to the temperature of 900-950 DEG C and maintaining for 20-30 minutes; (4) stopping heating, naturally cooling until the temperature is below 180 DEG C, taking out, carrying out air-cooling and then drying. The prepared activated carbon fiber cloth mainly comprises mesopores and also comprises micropores in an assisted manner, and is large in specific surface area and relatively high in yield.
Description
Technical field
The present invention relates to the preparation method of activated carbon fiber cloth, especially relate to the system of a kind of viscose base activated carbon fiber cloth
Preparation Method.
Background technology
Activated carbon fiber cloth is activated carbon fiber series newcomer, uses natural fiber cloth or Artificial Fibers cloth through pyrocarbon
Change, activation forms, and has the features such as specific surface area is big, pore is flourishing, absorbent properties are high, desorption rate is fast.It is widely used in molten
Agent recovery, air cleaning, water process, taste removal, deodorization, catalytic carrier, electrode material, health care, biochemical defence suit etc..Presently commercially available
Viscose base activated carbon fiber cloth based on micropore, its absorption aperture all concentrates on below 2nm, which limits it at big point
The application of sub-adsorbing domain, particularly in the application in the fields such as liquid phase adsorption, catalyst carrier, electronics, medical treatment.Therefore, micropore
Coordinate mesopore activated carbon fiber cloth research and development with produce become 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, it is provided that the system of a kind of viscose base activated carbon fiber cloth
Preparation Method, obtained activated carbon fiber cloth is based on mesopore and is aided with micropore, and specific surface area is big and yield is higher.
For reaching above-mentioned purpose, the technical scheme is that the preparation method of a kind of viscose base activated carbon fiber cloth, bag
Include following steps:
(1) select viscose rayon cloth be raw material, through distilled water clean after soak in acetone 3～5 hours for oil removing
And dehydration, then viscose rayon cloth is carried out room temperature and dry；
(2) putting in impregnation liquid by the viscose rayon cloth after step (1) processes, described impregnation liquid is chloride and sulphuric acid
Salt or phosphate or the mixture of nitrate, chloride is the one in sodium chloride, zinc chloride or potassium chloride, and sulfate is sulphuric acid
Ammonium, phosphate is the one in ammonium phosphate, ammonium dihydrogen phosphate or diammonium phosphate, and nitrate is in ammonium nitrate or magnesium nitrate
Kind, the total concentration of impregnation liquid controls 12～16wt%, and the most muriatic concentration is 5～9wt%, is first laid by viscose rayon
Entering in impregnation liquid 5～10 hours, then heat impregnation liquid with the intensification of 1 DEG C/min, impregnation liquid controls 80 the most at last
～the temperature 5 of 95 DEG C～after 8 hours take out viscose rayon cloth dry, dry temperature control at 125～140 DEG C；
(3) carbonizing apparatus will be sent into through the viscose rayon cloth after step (2) processes, carbonizing apparatus be passed through nitrogen, with 5
DEG C/programming rate of min to 250～300 DEG C and keeps 15 minutes, and protect to 500～600 DEG C with the programming rate of 8 DEG C/min
Hold 15 minutes, after 750～850 DEG C, be passed through carbon dioxide with the programming rate of 5 DEG C/min, keep 15～20 minutes, then lead to
Enter carbon dioxide and the gaseous mixture of steam and keep 20～30 minutes to 900～950 DEG C with the programming rate of 8 DEG C/min, mixed
Closing the mass values of carbon dioxide and steam in gas is 1:4～1:2；
(4) stop heating, stop logical carbon dioxide and the gaseous mixture of steam, continue to keep logical nitrogen, naturally cool to
Less than 180 DEG C taking-ups carry out air-cooled post-drying.
Described viscose rayon cloth is the knitting plain weave or twill, cloth weaved for primary raw material with long filament viscose rayon
Weight be 200-700g/m2。
The invention has the beneficial effects as follows: be first passed through carbon dioxide, contribute to the formation of micropore, after be passed through carbon dioxide and water
The gaseous mixture of steam passing ratio and temperature control so that a part of micropore is changed into mesopore, obtained activated carbon fiber
Cloth is based on mesopore and is aided with micropore, and specific surface area is big and yield is higher.
Detailed description of the invention
Below by embodiment, technical scheme is described in further detail.
Embodiment 1:
The preparation method of a kind of viscose base activated carbon fiber cloth, comprises the following steps:
(1) selecting viscose rayon cloth is raw material, and described viscose rayon cloth is to weave with long filament viscose rayon for primary raw material
Knitting plain, the weight of cloth is 200g/m2, through distilled water clean after soak in acetone 3 hours for oil removing
And dehydration, then viscose rayon cloth is carried out room temperature and dry；
(2) putting in impregnation liquid by the viscose rayon cloth after step (1) processes, described impregnation liquid is sodium chloride and sulphuric acid
The mixture of ammonium, the total concentration of impregnation liquid controls at 12wt%, and wherein the concentration of sodium chloride is 5wt%, first by viscose rayon cloth
Putting in impregnation liquid 5 hours, then heat impregnation liquid with the intensification of 1 DEG C/min, impregnation liquid controls at 80 DEG C the most at last
Temperature take out viscose rayon cloth after 5 hours and dry, dry temperature and control at 125 DEG C；
(3) carbonizing apparatus will be sent into through the viscose rayon cloth after step (2) processes, carbonizing apparatus be passed through nitrogen, with 5
DEG C/programming rate of min to 250 DEG C and keeps 15 minutes, and keep 15 minutes to 500 DEG C with the programming rate of 8 DEG C/min, with
The programming rate of 5 DEG C/min is passed through carbon dioxide after 750 DEG C, keeps 15 minutes, then passes to carbon dioxide and steam
Gaseous mixture also keeps 20 minutes to 900 DEG C with the programming rate of 8 DEG C/min, carbon dioxide and the mass ratio of steam in gaseous mixture
Value is 1:4；
(4) stop heating, stop logical carbon dioxide and the gaseous mixture of steam, continue to keep logical nitrogen, naturally cool to
Less than 180 DEG C taking-ups carry out air-cooled post-drying.
The specific surface area of obtained viscose base activated carbon fiber cloth is 980m2/ g, yield is 32%, and the aperture of mesopore is
24nm, the aperture of micropore is 0.6nm, and wherein mesopore accounts for 64%, and remainder is micropore.
Embodiment 2:
(1) selecting viscose rayon cloth is raw material, and described viscose rayon cloth is to weave with long filament viscose rayon for primary raw material
Knitting twill, the weight of cloth is 300g/m2, through distilled water clean after soak in acetone 3.5 hours for removing
Oil and dehydration, then carry out room temperature to viscose rayon cloth and dry；
(2) putting in impregnation liquid by the viscose rayon cloth after step (1) processes, described impregnation liquid is zinc chloride and phosphoric acid
The mixture of ammonium, the total concentration of impregnation liquid controls at 13wt%, and wherein chlorination zinc concentration is 6wt%, first by viscose rayon cloth
Putting in impregnation liquid 6 hours, then heat impregnation liquid with the intensification of 1 DEG C/min, impregnation liquid controls at 85 DEG C the most at last
Temperature take out viscose rayon cloth after 6 hours and dry, dry temperature and control at 130 DEG C；
(3) carbonizing apparatus will be sent into through the viscose rayon cloth after step (2) processes, carbonizing apparatus be passed through nitrogen, with 5
DEG C/programming rate of min to 260 DEG C and keeps 15 minutes, and keep 15 minutes to 520 DEG C with the programming rate of 8 DEG C/min, with
The programming rate of 5 DEG C/min is passed through carbon dioxide after 780 DEG C, keeps 16 minutes, then passes to carbon dioxide and steam
Gaseous mixture also keeps 22 minutes to 910 DEG C with the programming rate of 8 DEG C/min, carbon dioxide and the mass ratio of steam in gaseous mixture
Value is 1:3；
(4) stop heating, stop logical carbon dioxide and the gaseous mixture of steam, continue to keep logical nitrogen, naturally cool to
Less than 180 DEG C taking-ups carry out air-cooled post-drying.
The specific surface area of obtained viscose base activated carbon fiber cloth is 1290m2/ g, yield is 36%, the aperture of mesopore
For 28nm, the aperture of micropore is 0.8nm, and wherein mesopore accounts for 70%, and remainder is micropore.
Embodiment 3:
(1) selecting viscose rayon cloth is raw material, and described viscose rayon cloth is to weave with long filament viscose rayon for primary raw material
Knitting plain, the weight of cloth is 400g/m2.Through distilled water clean after soak in acetone 4 hours for oil removing
And dehydration, then viscose rayon cloth is carried out room temperature and dry；
(2) putting in impregnation liquid by the viscose rayon cloth after step (1) processes, described impregnation liquid is potassium chloride and phosphoric acid
The mixture of ammonium dihydrogen, the total concentration of impregnation liquid controls at 15wt%, and wherein the concentration of potassium chloride is 8wt%, first that viscose glue is fine
Wei Bu puts in impregnation liquid 8 hours, then heats impregnation liquid with the intensification of 1 DEG C/min, and impregnation liquid controls the most at last
The temperature of 90 DEG C takes out viscose rayon cloth after 7 hours dries, and dries temperature and controls at 135 DEG C；
(3) carbonizing apparatus will be sent into through the viscose rayon cloth after step (2) processes, carbonizing apparatus be passed through nitrogen, with 5
DEG C/programming rate of min to 280 DEG C and keeps 15 minutes, and keep 15 minutes to 570 DEG C with the programming rate of 8 DEG C/min, with
The programming rate of 5 DEG C/min is passed through carbon dioxide after 820 DEG C, keeps 18 minutes, then passes to carbon dioxide and steam
Gaseous mixture also keeps 27 minutes to 930 DEG C with the programming rate of 8 DEG C/min, carbon dioxide and the mass ratio of steam in gaseous mixture
Value is 1:2；
(4) stop heating, stop logical carbon dioxide and the gaseous mixture of steam, continue to keep logical nitrogen, naturally cool to
Less than 180 DEG C taking-ups carry out air-cooled post-drying.
The specific surface area of obtained viscose base activated carbon fiber cloth is 1670m2/ g, yield is 38%, the aperture of mesopore
For 40nm, the aperture of micropore is 1nm, and wherein mesopore accounts for 72%, and remainder is micropore.
Embodiment 4:
(1) selecting viscose rayon cloth is raw material, and described viscose rayon cloth is to weave with long filament viscose rayon for primary raw material
Knitting twill, the weight of cloth is 600g/m2, through distilled water clean after soak in acetone 5 hours for oil removing
And dehydration, then viscose rayon cloth is carried out room temperature and dry；
(2) putting in impregnation liquid by the viscose rayon cloth after step (1) processes, described impregnation liquid is sodium chloride and phosphoric acid
The mixture of hydrogen diammonium, the total concentration of impregnation liquid controls at 16wt%, and wherein the concentration of sodium chloride is 9wt%, first that viscose glue is fine
Wei Bu puts in impregnation liquid 10 hours, then heats impregnation liquid with the intensification of 1 DEG C/min, and impregnation liquid controls the most at last
The temperature of 95 DEG C takes out viscose rayon cloth after 8 hours dries, and dries temperature and controls at 140 DEG C；
(3) carbonizing apparatus will be sent into through the viscose rayon cloth after step (2) processes, carbonizing apparatus be passed through nitrogen, with 5
DEG C/programming rate of min to 300 DEG C and keeps 15 minutes, and keep 15 minutes to 600 DEG C with the programming rate of 8 DEG C/min, with
The programming rate of 5 DEG C/min is passed through carbon dioxide after 850 DEG C, keeps 20 minutes, then passes to carbon dioxide and steam
Gaseous mixture also keeps 30 minutes to 950 DEG C with the programming rate of 8 DEG C/min, carbon dioxide and the mass ratio of steam in gaseous mixture
Value is 1:2；
(4) stop heating, stop logical carbon dioxide and the gaseous mixture of steam, continue to keep logical nitrogen, naturally cool to
Less than 180 DEG C taking-ups carry out air-cooled post-drying.
The specific surface area of obtained viscose base activated carbon fiber cloth is 1950m2/ g, yield is 33%, the aperture of mesopore
For 38nm, the aperture of micropore is 1.2nm, and wherein mesopore accounts for 77%, and remainder is micropore.
Embodiment 5:
(1) selecting viscose rayon cloth is raw material, and described viscose rayon cloth is to weave with long filament viscose rayon for primary raw material
Knitting plain, the weight of cloth is 700g/m2, through distilled water clean after soak in acetone 4.5 hours for removing
Oil and dehydration, then carry out room temperature to viscose rayon cloth and dry；
(2) putting in impregnation liquid by the viscose rayon cloth after step (1) processes, described impregnation liquid is zinc chloride and nitric acid
The mixture of ammonium, the total concentration of impregnation liquid controls at 15wt%, and wherein chlorination zinc concentration is 7wt%, first by viscose rayon cloth
Putting in impregnation liquid 9 hours, then heat impregnation liquid with the intensification of 1 DEG C/min, impregnation liquid controls at 90 DEG C the most at last
Temperature take out viscose rayon cloth after 7.5 hours and dry, dry temperature and control at 136 DEG C；
(3) carbonizing apparatus will be sent into through the viscose rayon cloth after step (2) processes, carbonizing apparatus be passed through nitrogen, with 5
DEG C/programming rate of min to 285 DEG C and keeps 15 minutes, and keep 15 minutes to 570 DEG C with the programming rate of 8 DEG C/min, with
The programming rate of 5 DEG C/min is passed through carbon dioxide after 840 DEG C, keeps 19 minutes, then passes to carbon dioxide and steam
Gaseous mixture also keeps 28 minutes to 930 DEG C with the programming rate of 8 DEG C/min, carbon dioxide and the mass ratio of steam in gaseous mixture
Value is 1:2.5；
(4) stop heating, stop logical carbon dioxide and the gaseous mixture of steam, continue to keep logical nitrogen, naturally cool to
Less than 180 DEG C taking-ups carry out air-cooled post-drying.
The specific surface area of obtained viscose base activated carbon fiber cloth is 2020m2/ g, yield is 35%, the aperture of mesopore
For 44nm, the aperture of micropore is 0.9nm, and wherein mesopore accounts for 69%, and remainder is micropore.
Embodiment 6:
(1) selecting viscose rayon cloth is raw material, and described viscose rayon cloth is to weave with long filament viscose rayon for primary raw material
Knitting twill, the weight of cloth is 650g/m2, through distilled water clean after soak in acetone 4 hours for oil removing
And dehydration, then viscose rayon cloth is carried out room temperature and dry；
(2) putting in impregnation liquid by the viscose rayon cloth after step (1) processes, described impregnation liquid is potassium chloride and nitric acid
The mixture of magnesium, the total concentration of impregnation liquid controls at 14.8wt%, and wherein the concentration of potassium chloride is 7.6wt%, first that viscose glue is fine
Wei Bu puts in impregnation liquid 7.5 hours, then heats impregnation liquid with the intensification of 1 DEG C/min, and impregnation liquid controls the most at last
After the temperature 6 hours of 90 DEG C, take out viscose rayon cloth dry, dry temperature and control at 133 DEG C；
(3) carbonizing apparatus will be sent into through the viscose rayon cloth after step (2) processes, carbonizing apparatus be passed through nitrogen, with 5
DEG C/programming rate of min to 295 DEG C and keeps 15 minutes, and keep 15 minutes to 550 DEG C with the programming rate of 8 DEG C/min, with
The programming rate of 5 DEG C/min is passed through carbon dioxide after 815 DEG C, keeps 18 minutes, then passes to carbon dioxide and steam
Gaseous mixture also keeps 26 minutes to 910 DEG C with the programming rate of 8 DEG C/min, carbon dioxide and the mass ratio of steam in gaseous mixture
Value is 1:3；
(4) stop heating, stop logical carbon dioxide and the gaseous mixture of steam, continue to keep logical nitrogen, naturally cool to
Less than 180 DEG C taking-ups carry out air-cooled post-drying.
The specific surface area of obtained viscose base activated carbon fiber cloth is 1760m2/ g, yield is 47%, the aperture of mesopore
For 33nm, the aperture of micropore is 1nm, and wherein mesopore accounts for 71%, and remainder is micropore.
The foregoing is only the present invention preferably detailed description of the invention, but protection scope of the present invention be not limited thereto,
Any those familiar with the art in the technical scope that the invention discloses, the change that can readily occur in or replacement,
All should contain within protection scope of the present invention.
Claims (2)
1. the preparation method of a viscose base activated carbon fiber cloth, it is characterised in that: comprise the following steps:
(1) selecting viscose rayon cloth is raw material, soaks and within 3～5 hours, for oil removing and take off in acetone after distilled water cleans
Water, then carries out room temperature to viscose rayon cloth and dries；
(2) the viscose rayon cloth after step (1) processes is put in impregnation liquid, described impregnation liquid be chloride and sulfate or
Phosphate or the mixture of nitrate, chloride is the one in sodium chloride, zinc chloride or potassium chloride, and sulfate is ammonium sulfate,
Phosphate is the one in ammonium phosphate, ammonium dihydrogen phosphate or diammonium phosphate, and nitrate is the one in ammonium nitrate or magnesium nitrate,
The total concentration of impregnation liquid controls 12～16wt%, and the most muriatic concentration is 5～9wt%, is first put into by viscose rayon cloth
In impregnation liquid 5～10 hours, then impregnation liquid is heated with the intensification of 1 DEG C/min, the most at last impregnation liquid control 80～
The temperature 5 of 95 DEG C～after 8 hours take out viscose rayon cloth dry, dry temperature control at 125～140 DEG C；
(3) will through step (2) process after viscose rayon cloth send into carbonizing apparatus, carbonizing apparatus be passed through nitrogen, with 5 DEG C/
The programming rate of min is to 250～300 DEG C and keeps 15 minutes, to 500～600 DEG C and keeps 15 with the programming rate of 8 DEG C/min
Minute, after 750～850 DEG C, it is passed through carbon dioxide with the programming rate of 5 DEG C/min, keeps 15～20 minutes, then pass to two
Carbonoxide and the gaseous mixture of steam also keep 20～30 minutes to 900～950 DEG C with the programming rate of 8 DEG C/min, gaseous mixture
The mass values of middle carbon dioxide and steam is 1:4～1:2；
(4) stop heating, stop logical carbon dioxide and the gaseous mixture of steam, continue to keep logical nitrogen, naturally cool to 180 DEG C
Hereinafter take out and carry out air-cooled post-drying.
The preparation method of a kind of viscose base activated carbon fiber cloth the most as claimed in claim 1, it is characterised in that: described viscose rayon
Cloth is the knitting plain weave or twill weaved for primary raw material with long filament viscose rayon, and the weight of cloth is 200-700g/m2。
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| CN108950739A (en) * | 2017-12-29 | 2018-12-07 | 海南梵思科技有限公司 | A kind of preparation method of carbon fiber and high-temperature nylon composite material containing it |
| CN109972235A (en) * | 2019-03-22 | 2019-07-05 | 武汉工程大学 | A kind of preparation method of activated carbon fiber |
| CN113060726A (en) * | 2021-03-25 | 2021-07-02 | 河南理工大学 | Viscose-based nitrogen-containing activated carbon fiber material and preparation method and application thereof |
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Application publication date: 20161026 |
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