CN1102675C - Air activating process for preparing activated carbon fibres - Google Patents
Air activating process for preparing activated carbon fibres Download PDFInfo
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- CN1102675C CN1102675C CN00130714A CN00130714A CN1102675C CN 1102675 C CN1102675 C CN 1102675C CN 00130714 A CN00130714 A CN 00130714A CN 00130714 A CN00130714 A CN 00130714A CN 1102675 C CN1102675 C CN 1102675C
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Abstract
The present invention relates to a method for preparing activated carbon fibres by activation with air, which comprises the two steps of carbonization and activation, wherein the step of activation adopts air as an activating agent and is carried out for 20 to 90 min at 400 to 500 DEG C with air mass flow of 10 to 50 ml/min. g. The method can be carried out continuously or intermittently. Compared with the prior art, the present invention has the advantages of low energy consumption, low cost and short preparation periodicity.
Description
The invention belongs to the preparation method of activated carbon fiber, be specifically related to a kind of air-activated method for preparing activated carbon fiber.
Activated carbon fiber has particular structure and performance characteristic, has a wide range of applications in fields such as chemical industry, environmental protection, defence and military, electronics and the energy, has caused people's attention since 1960's comes out always, is developed rapidly about the seventies.The preparation method of activated carbon fiber also is one of emphasis problem of different researcher's extensive concerns always.But for a long time,, restricted its application in all many-sides because the cost and price of activated carbon fiber own is higher.Different preparation method itself may cause the final products activated carbon fiber to have different pore structures and surface group, so that improve the adsorption efficiency and the adsorptive selectivity of activated carbon fiber.Traditional preparation method (Yoshida A.USP4814145 1989) is divided into charing and two steps of activation, and its activation method generally is to adopt steam or carbon dioxide to carry out charing and activation under the protection of nitrogen or argon gas.The preparation method who adopts protection gas is the cost height not only, and reaction occurs in 800-1000 ℃ high temperature, and energy consumption is bigger, is difficult for the occasion that obtains or lack for protection gas, can cause the inconvenience of producing and using.
The objective of the invention is to develop a kind of power consumption less, the cost air-activated method for preparing activated carbon fiber low, with short production cycle.
The present invention prepares the method for activated carbon fiber and also is made up of charing and activation, it is characterized in that described activation employing air as activator, and activation temperature is 400-500 ℃, and air mass flow is a 10-50ml/ming charcoal fiber, soak time 20-90min.
Method of the present invention can be intermittently, can also be continuous.
The step of batch process is as follows:
(1) fibrous raw material for the treatment of charing is in retort, and under protection of nitrogen gas, 800-1000 ℃ is carried out charing;
(2) the charcoal fiber after the charing is directly put into the activation furnace that has been heated to 400-500 ℃, control air mass flow 10-50ml/ming charcoal fiber, activation 20-90min gets the product activated carbon fiber.
The step of continuity method is as follows:
(1) fibrous raw material for the treatment of charing is full of nitrogen continuously by retort in the stove, carries out charing under 800-1000 ℃;
(2) the charcoal fiber that constantly comes out from retort enters activation furnace, and the flow velocity of control air is a 10-50ml/ming charcoal fiber, activates 20-90min continuously, gets the product activated carbon fiber.
Described fibrous raw material is viscose, polyacrylonitrile fibre, it can also be made different shapes such as felt, cloth, paper.
Control the reaction temperature of activation and the flow velocity of activator air, can obtain the product of different structure and performance.
The conspicuous advantage of the present invention is: owing to using air to replace in the past steam and carbon dioxide as activator, and be reflected under the lower temperature and carry out, not only reduce production costs, and minimizing energy consumption, the product that obtained also has with steam, carbon dioxide in the past activate the different pore structure of gained sample simultaneously, even also can be near continous mode production for its whole process of production of Batch Process equipment.Because need not image height temperature activation in the production process cools off under protective atmosphere like that and sample could be taken out then; production cycle is longer relatively; just can take out sample at once and add raw material as long as reach required soak time simultaneously, and the production of beginning next round, the production cycle shortens.
Embodiment 1
About 10g charcoal fiber is directly put into the activation furnace that has been heated to 400 ℃, and the bubbling air amount is 50ml/ming, and reaction time 20min, the yield of gained activated carbon fiber are 53.49%, and the benzene adsorbance is 211.41mg/g.
Embodiment 2
450 ℃ of reaction temperatures, air mass flow 45ml/ming, the reaction time is 30min, and the yield of product activated carbon fiber is 40.36%, and the BET specific area is 375m
2/ g, the benzene adsorbance is 199.23mg/g, other are with embodiment 1.
Embodiment 3
400 ℃ of reaction temperatures, air mass flow 45ml/ming, the reaction time is 60min, and the yield of product activated carbon fiber is 33.41%, and the BET specific area is 450m
2/ g, the benzene adsorbance is 234.34mg/g, other are with embodiment 1.
Embodiment 4
400 ℃ of reaction temperatures, air mass flow 50ml/ming, the reaction time is 90min, and the yield of product activated carbon fiber is 21.22%, and the BET specific area is 530m
2/ g, the benzene adsorbance is 287.17mg/g, other are with embodiment 1.
Embodiment 5
The charcoal fiber is passed through activation furnace, 450 ℃ of control reaction temperature, reaction time 60min, air mass flow 10ml/ming, the yield 41.41% of products obtained therefrom activated carbon fiber, benzene adsorbance 185.41mg/g continuously.
Embodiment 6
Reaction time 40min, air mass flow 20ml/ming, yield 29.15%, benzene adsorbance 253.23mg/g, other are with embodiment 5.
Embodiment 7
Reaction time 20min, air mass flow 30ml/ming, yield 26.2%, benzene adsorbance 265.34mg/g, other are with embodiment 5.
Embodiment 8
Reaction time 10min, air mass flow 50ml/ming, yield 30.23%, benzene adsorbance 265.54mg/g, other are with embodiment 5.
Although the specific area by air-activated results sample is very not high, its sample is to the absorption and the steam activation sample (S of benzene
BBT=750m
2/ g) static benzene adsorbance (the benzene adsorbance is 245mg/g) is suitable.The latter more has Practical significance.
Comparative Examples 1: adopt the polyacrylonitrile raw material identical with embodiment 4,820 ℃ with the steam activation of routine 2 hours, the yield of gained sample is 22%, the BET specific area is 860m
2/ g, the pore-size distribution of the sample that this Comparative Examples and embodiment 4 are obtained compares, and the result is as shown in Figure 1.Wherein a is embodiment 4 samples, and b is Comparative Examples 1 sample.Has suitable ablation degree though this shows two kinds of samples, but the specific area by the air-activated sample that obtains is also not really high, its pore size distribution range is but very narrow, almost most distribution of pores and have complicated pore-size distribution with the activated carbon fiber sample of steam activation below 1nm.Also can obviously find out to have the pore-size distribution of quite concentrating for air-activated sample from figure, such pore-size distribution may make it be suitable for selective absorption.
Comparative Examples 2: adopt the polyacrylonitrile raw material identical with embodiment 4, at 820 ℃ of steam activations with routine, the BET specific area is 750m
2/ g.Since the chemism of oxygen than steam and carbon dioxide be eager to excel many, and under lower reaction temperature, easily and carbon surface form the stable oxygen surface functional group that contains.As everyone knows, surface functional group and pore structure have the influence of no less important to adsorption process.The existence of surface functional group with the absorption that influences to a great extent polar substances, particularly is easy to form the material of hydrogen bond such as steam, alcohol, ammonia etc.The comparative result that is the activated carbon fiber sample of different activator activation to ethanol absorption as shown in the table, the sample with air-activated preparation has higher adsorptive selectivity to ethanol as can be seen, further specifies the effect of surface functional group thus.
| Sample | The steam activation sample | Air-activated sample |
| 750m 2/g | 530m 2/g | |
| Ethanol adsorbance (mg/g) | 235 | 280 |
Claims (3)
1. an air-activated method for preparing the charcoal fiber is made of with activating for two steps charing, it is characterized in that it is activator that air is adopted in described activation, and activation temperature is 400-500 ℃, and air mass flow is a 10-50ml/ming charcoal fiber, soak time 20-90min.
2. the method for claim 1 is characterized in that described activation can be intermittently, can also be continuous.
3. as the method for claim 1 or 2, it is characterized in that described charing raw material is viscose or polyacrylonitrile fibre, can also be felt, cloth or the paper of described fiber.
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| Application Number | Priority Date | Filing Date | Title |
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| CN00130714A CN1102675C (en) | 2000-10-11 | 2000-10-11 | Air activating process for preparing activated carbon fibres |
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| Application Number | Priority Date | Filing Date | Title |
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| CN00130714A CN1102675C (en) | 2000-10-11 | 2000-10-11 | Air activating process for preparing activated carbon fibres |
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| CN1305025A CN1305025A (en) | 2001-07-25 |
| CN1102675C true CN1102675C (en) | 2003-03-05 |
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| CN00130714A Expired - Fee Related CN1102675C (en) | 2000-10-11 | 2000-10-11 | Air activating process for preparing activated carbon fibres |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1109140C (en) * | 2000-10-28 | 2003-05-21 | 中山大学 | Phosphoric acid activation process of producing active carbon fiber |
| CN105862250A (en) * | 2016-05-16 | 2016-08-17 | 上海申欧企业发展有限公司 | Active carbon composite cloth and preparation process and application thereof |
| CN109894077A (en) * | 2018-12-28 | 2019-06-18 | 安徽天富环保科技材料有限公司 | A kind of viscose base activated carbon fiber high-temperature activation device and method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4699896A (en) * | 1984-09-11 | 1987-10-13 | The Secretary Of State For Defence In Her Britannic Majesty's Government Of The United Kingdom Of Great Britain And Northern Ireland | Manufacture of fibrous activated carbons |
| CN1115796A (en) * | 1994-07-28 | 1996-01-31 | 刘智仁 | Prepn of high-adsorption active carbon fibre |
| CN1166541A (en) * | 1997-04-18 | 1997-12-03 | 中山大学 | Preparation method of natural fibre-based active carbon fibre |
| CN1238395A (en) * | 1999-06-11 | 1999-12-15 | 中山大学 | Process for preparing activated carbon fibres by boric acid activating method |
| CN1295142A (en) * | 2000-10-28 | 2001-05-16 | 中山大学 | Phosphoric acid activation process of producing active carbon fiber |
| CN1303963A (en) * | 2000-07-21 | 2001-07-18 | 中国科学院山西煤炭化学研究所 | Method for preparing foam block active carbon fibre |
-
2000
- 2000-10-11 CN CN00130714A patent/CN1102675C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4699896A (en) * | 1984-09-11 | 1987-10-13 | The Secretary Of State For Defence In Her Britannic Majesty's Government Of The United Kingdom Of Great Britain And Northern Ireland | Manufacture of fibrous activated carbons |
| CN1115796A (en) * | 1994-07-28 | 1996-01-31 | 刘智仁 | Prepn of high-adsorption active carbon fibre |
| CN1166541A (en) * | 1997-04-18 | 1997-12-03 | 中山大学 | Preparation method of natural fibre-based active carbon fibre |
| CN1238395A (en) * | 1999-06-11 | 1999-12-15 | 中山大学 | Process for preparing activated carbon fibres by boric acid activating method |
| CN1303963A (en) * | 2000-07-21 | 2001-07-18 | 中国科学院山西煤炭化学研究所 | Method for preparing foam block active carbon fibre |
| CN1295142A (en) * | 2000-10-28 | 2001-05-16 | 中山大学 | Phosphoric acid activation process of producing active carbon fiber |
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