CN1114729C - Preparation method of foam block active carbon fibre - Google Patents
Preparation method of foam block active carbon fibre Download PDFInfo
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- CN1114729C CN1114729C CN 00104483 CN00104483A CN1114729C CN 1114729 C CN1114729 C CN 1114729C CN 00104483 CN00104483 CN 00104483 CN 00104483 A CN00104483 A CN 00104483A CN 1114729 C CN1114729 C CN 1114729C
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- carbon fiber
- active carbon
- foam block
- activated carbon
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Abstract
The present invention relates to a method for preparing a foam blocky activated carbon fiber. An organic high molecular polymer, a cross linking agent, a foaming agent and a short-cutting activated carbon fiber or an activated carbon fiber powder are used as raw material, are stirred by certain proportion, are uniformly mixed, are pressed into blocks by dies, and are processed by preoxidization, carbonization and active treatment, and thus, the foam blocky activated carbon fiber is prepared. The present invention has the characteristic that the preparation technology is simple and is easy to operate; the foam blocky activated carbon fiber has good adsorption activity, high mechanical strength and high bulk density; the purifying equipment can be miniaturized.
Description
The invention belongs to a kind of preparation method of activated carbon fiber, relate in particular to a kind of preparation method of foam block active carbon fibre.
Activated carbon fiber is concentrated owing to having bigger specific area and abundant microporous structure and pore-size distribution, thereby as a kind of new and effective sorbing material, is subjected to the common concern of Chinese scholars.The active carbon fibre fiber products of having developed at present has several forms such as fiber, cloth, felt, paper, and they all have trace contaminant in the environment adsorbs capture ability preferably, all can be used in the purification and improvement engineering of trace contaminant in the sky G﹠W.As everyone knows, the absorption property of activated carbon fiber and its preparation raw material, technology are relevant with chemical constitution.Generally speaking, absorption property depends on its specific surface and microcellular structure, and specific area is big, and microcellular structure is abundant, and absorption property is good.But the intensity of Large ratio surface activated carbon fiber is relatively poor, is difficult to as a kind of engineering material.In addition, present existing active carbon fibre fiber products such as fiber, felt, cloth, paper etc. all exist the low shortcoming of bulk density.When for example the activated carbon fiber felt is as environment deodoring materials such as material for air purification and organic solvent salvage material and freezer, refrigerators, exist because of the huge problem of the low and required device of packed density.Installing huge shortcoming one is consumptive material expense height, the 2nd, taken expensive real estate.In addition, present existing active carbon fibre fiber products is when being used for the dynamic process of sky G﹠W, and the resistance to mass tranfer that also exists fluid is big, penetrates the shortcoming of difficulty.
Goal of the invention of the present invention provides the preparation method of a kind of intensity height, density is big and resistance to mass tranfer is little foam block active carbon fibre.
The object of the present invention is achieved like this: adopting organic polymer, crosslinking agent, blowing agent and short activated carbon fiber or the activated carbon fiber powder of cutting is raw material, after mixing by a certain percentage, be molded into block, through pre-oxidation, charing and active the processing, make foam block active carbon fibre again.
Concrete preparation method of the present invention is as follows:
(1) with liquid organic polymer or SOLID ORGANIC high polymeric solution, crosslinking agent and blowing agent be by weight: organic polymer: blowing agent: crosslinking agent=2-20: 0.1-20: 1 composition mixes, and obtains the high polymeric solution mixture;
(2) activated carbon fiber or the activated carbon fiber powder with 0.5 to 5 millimeters long is by weight: activated carbon fiber or activated carbon fiber powder: high polymeric solution=1-10: 1 ratio joins in the high polymeric solution mixture, mix, obtain mixture;
(3) mixture is put into mould, be heated to 80-240 ℃, solidified 20-240 minute, obtain the foam block thing;
(4) the foam block thing is placed retort, the heating rate by 1-30 ℃/minute in air is warmed up to 200-300 ℃, and pre-oxidation 5-240 minute, feed inert gas then and under inert gas shielding, be warmed up to 600-1000 ℃, carried out charing 5-240 minute;
(5) after charing is handled, feed activator and activate 10-120 minute, activation is cooled to 100 ℃ after finishing under inert atmosphere, make foam block active carbon fibre.
Aforesaid organic polymer is phenolic resins, pitch, epoxy resin, polyurethane, base polyurethane prepolymer for use as solution, polyvinyl alcohol.
Aforesaid organic amine crosslinking agent is a diethylentriamine, triethylenetetramine, phenylenediamine, dicyandiamide, 2-ethyl diethylentriamine, dimethylamino methyl phenol.
Aforesaid organic peroxide crosslinking agent is a cyclohexanone peroxide, 2, and 5-dimethyl-2, two (tert-butyl peroxy base) hexanes of 5-, cumyl peroxide, benzoyl peroxide, peroxidating tert-butyl acetate.
Aforesaid blowing agent is sulfohydrazide type blowing agents such as azo foaming agent, benzene sulfonyl hydrazide such as ammonium hydrogencarbonate, sodium bicarbonate, blowing agent A-C, blowing agent H.
Aforesaid activated carbon fiber is phenolic resin based activated carbon fiber, asphalt based active carbon fiber, viscose-based active carbon fiber, polyacrylonitrile radical active carbon fiber, polyvinyl alcohol-based active carbon fiber.
Aforesaid activator is steam, carbon dioxide gas, ammonia.
Foam block active carbon fibre of the present invention can be widely applied to the purification and the improvement field of environmental pollution.
The present invention compared with prior art has following advantage:
(1) preparation technology is simple, and is easy to operate;
(2) have good adsorption activity and mechanical strength;
(3) have higher bulk density, can make the cleaning equipment miniaturization.
Embodiments of the invention are as follows:
Embodiment 1
20 gram phenolic resins are dissolved in 30 milliliters of ethanol, add 2 gram six methines, four ammonia and 1 gram 2, the 2-azodiisobutyronitrile stirs and makes Polymer Solution.With 40 gram polyacrylonitrile radical active carbon fiber felt grind into powders, add in the above-mentioned high polymer mixture solution stir make mix after, put into iron mould compacting, behind 70 ℃ of volatilization alcohol solvents, be heated to 180 ℃, keep this temperature 20 minutes, and made the moulding of material foamed solidification, promptly obtain the foam block material.This bulk material is placed retort, and under nitrogen protection, the heating rate of spending with per minute 5 is warmed up to 800 ℃, and charing 100 minutes fed steam activation 20 minutes then, when cooling to 150 ℃, can obtain the rigid foam block active carbon fibre.Adsorption experiment shows that this material is suitable to the adsorption effect and the activated carbon fiber of organic vapors such as benzene.Because this material has abundant open celled foam, fluid breathability is good, and intensity is also higher, thereby is suitable as very much the filtering material of air and water treatment.
Embodiment 2
10 gram epoxy resin are dissolved in 10 milliliters of acetone solns, add 4 gram dimethylaminopropylamine and 0.1 gram blowing agent H, stir and make the high polymer mixture solution.40 gram viscose-based active carbon fiber weak points are cut into the short silk that length is the 4-5 millimeter, join in the above-mentioned high polymer mixture solution stir make mix after, put into iron mould, behind 70 ℃ of solvent flashings, be heated to 200 ℃, keep this temperature 120 minutes, and made the moulding of material foamed solidification, promptly obtain steeping last bulk material.This bulk material is placed retort, and under nitrogen protection, the heating rate of spending with per minute 2 is warmed up to 850 ℃, and charing 30 minutes fed steam activation 60 minutes then, when cooling to 150 ℃, can obtain the rigid foam block active carbon fibre.Adsorption experiment shows that this material is suitable to the adsorption effect and the activated carbon fiber of organic vapors such as benzene.Because this material has abundant open celled foam, fluid breathability is good, and intensity is also higher, thereby is suitable as very much the filtering material of air and water treatment.
Embodiment 3
5 gram polyvinyl alcohol are dissolved in 10 ml waters, add 2 gram six methines, four ammonia and 5 gram ammonium hydrogencarbonates, stir and make the high polymer mixture solution.With 40 gram polyvinyl alcohol-based active carbon fiber felt grind into powders, add in the above-mentioned high polymer mixture solution stir make mix after, put into iron mould, compacting also is heated to 100 ℃, kept this temperature 20 minutes, solvent flashing and make the moulding of material foamed solidification promptly obtains steeping last bulk material.This bulk material is placed retort, and under protection of ammonia, the heating rate of spending with per minute 2 is warmed up to 900 ℃, and charing 10 minutes feeds carbon dioxide activation 10 minutes then, when cooling to 150 ℃, can obtain the rigid foam block active carbon fibre.Adsorption experiment shows that this material is suitable to the adsorption effect and the activated carbon fiber of organic vapors such as benzene.Because this material has abundant open celled foam, fluid breathability is good, and intensity is also higher, thereby is suitable as very much the filtering material of air and water treatment.
Embodiment 4 is dissolved in 20 gram base polyurethane prepolymer for use as in 30 milliliters of ethanol, and adds 5 gram organic amine crosslinking agent MOCA (3,3-two chloro-4,4-diaminodiphenyl-methane) and 2 gram blowing agent benzene sulfonyl hydrazides, stirs and makes the high polymer mixture solution.With 40 gram asphalt based active carbon fibrofelt grind into powders, add stir in the above-mentioned high polymer mixture solution make mix after, put into iron mould, behind 70 ℃ of solvent flashings, be heated to 200 ℃, kept this temperature 60 minutes, make the moulding of material foamed solidification, promptly obtain steeping last bulk material.This bulk material is placed retort, and under nitrogen protection, the heating rate of spending with per minute 15 is warmed up to 800 ℃, and charing 150 minutes fed ammonia activation 120 minutes, when cooling to 150 ℃, can obtain foam block active carbon fibre.
Embodiment 5
20 gram epoxy resin are dissolved in 10 milliliters of acetone solns, and add 10 gram phthalic anhydrides, stir and make the high polymer mixture solution.With 40 gram length is the phenolic resin based activated carbon fiber of 1-2mm, add in the above-mentioned high polymer mixture solution, add again 30 gram sodium bicarbonates stir make mix after, put into iron mould, behind 70 ℃ of solvent flashings, be heated to 200 ℃, kept this temperature 20 minutes, make the moulding of material foamed solidification, promptly obtain the foam block material.This bulk material is placed retort, and under nitrogen protection, the heating rate of spending with per minute 2 is warmed up to 600 ℃; charing 200 minutes is being warmed up to 800 ℃, feeds steam activation 100 minutes; when cooling to 150 ℃, can obtain the rigid foam block active carbon fibre.
Claims (8)
1. the preparation method of a foam block active carbon fibre:
(1) with liquid organic polymer or SOLID ORGANIC high polymeric solution, crosslinking agent and blowing agent be by weight: organic polymer: blowing agent: crosslinking agent=2-20: 0.1-20: 1 composition mixes, and obtains the high polymeric solution mixture;
(2) activated carbon fiber or the activated carbon fiber powder with 0.5 to 5 millimeters long is by weight: activated carbon fiber or activated carbon fiber powder: high polymeric solution=1-10: 1 ratio joins in the high polymeric solution mixture, mix, obtain mixture;
(3) mixture is put into mould, be heated to 80-240 ℃, solidified 20-240 minute, obtain the foam block thing;
(4) the foam block thing is placed retort, the heating rate by 1-30 ℃/minute in air is warmed up to 200-300 ℃, and pre-oxidation 5-240 minute, feed inert gas then and under inert gas shielding, be warmed up to 600-1000 ℃, carried out charing 5-240 minute;
(5) after charing is handled, feed activator and activate 10-120 minute, activation is cooled to 100 ℃ after finishing under inert atmosphere, make foam block active carbon fibre.
2. the preparation method of a kind of foam block active carbon fibre according to claim 1 is characterized in that described organic polymer is phenolic resins, pitch, epoxy resin, polyurethane, base polyurethane prepolymer for use as solution or polyvinyl alcohol.
3. the preparation method of a kind of foam block active carbon fibre according to claim 1 is characterized in that described crosslinking agent is six methines, four ammonia, hydrochloric acid, organic peroxide, amine, anhydrides or imidazoles.
4. the preparation method of a kind of foam block active carbon fibre according to claim 3 is characterized in that described peroxide is a cyclohexanone peroxide, 2; 5-dimethyl-2; two (tert-butyl peroxy base) hexane, cumyl peroxide, benzoyl peroxide or the peroxidating tert-butyl acetates of 5-.
5. the preparation method of a kind of foam block active carbon fibre according to claim 3 is characterized in that described amine is a diethylentriamine, triethylenetetramine, phenylenediamine, dicyandiamide, 2-ethyl diethylentriamine or dimethylamino methyl phenol.
6. the preparation method of a kind of foam block active carbon fibre according to claim 1 is characterized in that described blowing agent is ammonium hydrogencarbonate, sodium bicarbonate, blowing agent A-C, blowing agent H or benzene sulfonyl hydrazide.
7. the preparation method of a kind of foam block active carbon fibre according to claim 1 is characterized in that described activated carbon fiber is phenolic resin based activated carbon fiber, asphalt based active carbon fiber, viscose-based active carbon fiber, polyacrylonitrile radical active carbon fiber or polyvinyl alcohol-based active carbon fiber.
8. the preparation method of a kind of foam block active carbon fibre according to claim 1 is characterized in that activator is steam, carbon dioxide gas or ammonia.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00104483 CN1114729C (en) | 2000-07-21 | 2000-07-21 | Preparation method of foam block active carbon fibre |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00104483 CN1114729C (en) | 2000-07-21 | 2000-07-21 | Preparation method of foam block active carbon fibre |
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| CN1303964A CN1303964A (en) | 2001-07-18 |
| CN1114729C true CN1114729C (en) | 2003-07-16 |
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| CN 00104483 Expired - Fee Related CN1114729C (en) | 2000-07-21 | 2000-07-21 | Preparation method of foam block active carbon fibre |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491498B (en) * | 2011-12-16 | 2013-11-27 | 北京化工大学 | Ecological carbon-fiber composite, preparation method thereof and sewage treatment reactor containing ecological carbon-fiber composite |
| CN103159330B (en) * | 2013-04-07 | 2014-03-12 | 武汉钢铁(集团)公司 | Porous light-weight carbon-based biological carrier and preparation method thereof |
| CN106430179B (en) * | 2016-09-23 | 2018-11-23 | 郑州峰泰纳米材料有限公司 | A kind of mushroom source foam active Carbon Materials and preparation method thereof |
| KR102506938B1 (en) * | 2018-02-02 | 2023-03-07 | 현대자동차 주식회사 | Method for manufacturing activated carbon |
| CN108383101B (en) * | 2018-05-18 | 2019-12-10 | 山东大学 | Preparation method of polyacrylonitrile-based three-dimensional macroporous carbon block |
| CN113786822B (en) * | 2021-11-16 | 2022-02-22 | 因达孚先进材料(苏州)有限公司 | Preparation method of active carbon fiber loaded magnetic resin microsphere porous material |
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