CN1238395A - Process for preparing activated carbon fibres by boric acid activating method - Google Patents
Process for preparing activated carbon fibres by boric acid activating method Download PDFInfo
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- CN1238395A CN1238395A CN99116239A CN99116239A CN1238395A CN 1238395 A CN1238395 A CN 1238395A CN 99116239 A CN99116239 A CN 99116239A CN 99116239 A CN99116239 A CN 99116239A CN 1238395 A CN1238395 A CN 1238395A
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Abstract
A process for preparing activated carbon fibres by boric acid activating method includes such technological steps as immersing cellulose fibres as raw material in boric acid as carbonizing and activating agent, drying, and then carbonizing and activating in heating furnace for a certain time. Its advantages are simple process, high output rate, low cost and low content of impurities.
Description
The present invention relates to a kind of preparation method of activated carbon fiber.
Activated carbon fiber has flourishing specific surface and outstanding pore structure, and therefore high adsorption capacity has good prospects for application in fields such as environmental protection.Along with improving constantly of human environment consciousness, the production of this efficient adsorption and separation material and application and development work more and more cause people's attention.In recent years, the production technology and the equipment of activated carbon fiber constantly improve, and application technology constantly develops, and has created good environment and economic benefit.Yet most at present activated carbon fibers is still the method preparation of adopting steam activation, the carbonization-activation temperature that this arts demand is higher, and usually at 800 to 900 ℃, and the product yield is lower, usually at 14-20%.Therefore exist energy consumption bigger, the shortcoming that product cost is high.Recently, people have mainly carried out some researchs in the preparation technology of phosphoric acid activation sisal based activated carbon fiber, have obtained certain achievement.Though phosphoric acid activation preparation technology can improve the yield of products obtained therefrom greatly, the mechanical performance of fiber is relatively poor, and fragility is big, and Application Areas is restricted.In addition, the technology of phosphoric acid activation exists the pretreatment of fiber moisture absorption very big, and this gives depositing of production operation and material previously treated and management is made troubles.
It is easy to the purpose of this invention is to provide a kind of production operation, and the product flexibility is good, and activation temperature is low, the activated carbon fiber production technology that the product yield is high.
Method of the present invention is: it is fully moistening to place boric acid aqueous solution to be dipped to fiber the cellulose fibre raw material; pull out and wring out; low temperature (100 ℃) is done behaviour down; the heating carbonization-activation is 20 to 120 minutes under nitrogen protection; heating-up temperature is 350 to 800 ℃; naturally wash with water repeatedly after the cooling then, 110 to 120 ℃ of oven dry.In the methods of the invention, boric acid concentration is controlled at 2～15% or higher, but is conservation and reducing cost, and boric acid concentration needn't be too high.The time that raw fiber soaks boric acid is several hours to tens hours, to fiber fully moistening till.The load capacity of boric acid on raw fiber is controlled at 9～90wt%.
Take boric acid to soak fibrous raw material as the carbonization-activation agent, method is simple, processing ease, and particularly the carbonization-activation temperature is lower, and energy consumption is reduced greatly, and the product yield can reach more than 30%, and than all high with other method, and the product softness is good.
Fig. 1 is for adopting the pore size distribution curve of technology of the present invention at the activated carbon fiber of three kinds of different activation temperature preparations.
Fig. 2 is for adopting the aperture of technology of the present invention at the activated carbon fiber of three kinds of different activation temperature preparations--accumulation specific area relation curve.
Among Fig. 1, ordinate is pore volume (CC/g), and abscissa is aperture (), and B500, B700, B800 are respectively the pore size distribution curve of the activated carbon fiber of boric acid activation under 500,700,800 ℃ of temperature.The aperture of explanation product is mainly between 5～10 among the figure.
Among Fig. 2, the accumulation of ordinate is than the long-pending (m of table
2/ g).Abscissa is the aperture, and B500, B700, B800 are respectively the aperture and accumulation specific area relation curve of the activated carbon fiber of boric acid activation under 500,700,800 ℃ of temperature.The accumulation specific area of explanation product reaches 500～580m among the figure
2/ g.
The invention will be further described by the following examples:
Embodiment 1, get raw fiber 10.4 gram, with immersion in 200 milliliter of 2.5% BAS 24 hours, pull out, wring out, behind the low temperature drying, boric acid load capacity on raw fiber is 7.0wt%.Fiber after handling is positioned in the carbonization-activation stove, under nitrogen protection, is warming up to 500 ℃, reacted 90 minutes.Naturally cool then to room temperature, take out fiber and wash 120 ℃ of oven dry with water 5 times.The yield that records product is 35.7wt%, and specific area is 413 meters
2/ gram is to the 153 milligrams/gram of adsorbance of benzene vapour.
Embodiment 2, get raw fiber 8.0 gram, with immersion in 200 milliliter of 5% BAS 20 hours, pull out, wring out, behind the low temperature drying, boric acid load capacity on raw fiber is 31wt%.Fiber after handling is positioned in the carbonization-activation stove, under the chlorine protection, is warming up to 500 ℃, reacted 120 minutes.Naturally cool then to room temperature, take out fiber and wash 120 ℃ of oven dry with water 4 times.The yield that records product is 34.4wt%, and specific area is 505 meters
2/ gram is to the 189 milligrams/gram of adsorbance of benzene vapour.
Embodiment 3, get raw fiber 9.8 gram, with immersion in 200 milliliter of 7.5% BAS 2 hours, pull out, wring out, behind the low temperature drying, boric acid load capacity on raw fiber is 58wt%.Fiber after handling is positioned in the carbonization-activation stove, under nitrogen protection, is warming up to 500 ℃, reacted 20 minutes.Naturally cool then to room temperature, take out fiber and wash 120 ℃ of oven dry with water 4 times.The yield that records product is 38.6wt%, and specific area is 493 meters
2/ gram is to the 180 milligrams/gram of adsorbance of benzene vapour.
Embodiment 4, get raw fiber 11.4 gram, with immersion in 200 milliliter of 10% BAS 24 hours, pull out, wring out, behind the low temperature drying, boric acid load capacity on raw fiber is 88wt%.Fiber after handling is positioned in the carbonization-activation stove, under nitrogen protection, is warming up to 500 ℃, reacted 90 minutes.Naturally cool then to room temperature, take out fiber and wash 120 ℃ of oven dry with water 3 times.The yield that records product is 37.1wt%, and specific area is 465 meters
2/ gram is to the 187 milligrams/gram of adsorbance of benzene vapour.
Embodiment 5, get raw fiber 9.61 gram, with immersion in 200 milliliter of 12.5% BAS 10 hours, pull out, wring out, behind the low temperature drying, boric acid load capacity on raw fiber is 26wt%.Fiber after handling is positioned in the carbonization-activation stove, under nitrogen protection, is warming up to 500 ℃, reacted 90 minutes.Naturally cool then to room temperature, take out fiber and wash 120 ℃ of oven dry with water 5 times.The yield that records product is 34.2wt%, to the 200 milligrams/gram of adsorbance of benzene vapour.
Embodiment 6, get raw fiber 8.88 gram, with immersion in 200 milliliter of 6.2% BAS 20 hours, pull out, wring out, behind the low temperature drying, boric acid load capacity on raw fiber is 9.0wt%.Fiber after handling is positioned in the carbonization-activation stove, under nitrogen protection, is warming up to 350 ℃, reacted 90 minutes.Naturally cool then to room temperature, take out fiber and wash 120 ℃ of oven dry with water 4 times.The yield that records product is 46.9wt%, to the 59 milligrams/gram of adsorbance of benzene vapour.
Embodiment 7, get raw fiber 11.4 gram, with immersion in 200 milliliter of 6.2% BAS 15 hours, pull out, wring out, behind the low temperature drying, boric acid load capacity on raw fiber is 9.0wt%.Fiber after handling is positioned in the carbonization-activation stove, under the chlorine protection, is warming up to 700 ℃, reacted 90 minutes.Naturally cool then to room temperature, take out fiber and wash 120 ℃ of oven dry with water 5 times.The yield that records product is 32.5wt%, and more long-pending than table is 499 meters
2/ gram is to the 206 milligrams/gram of adsorbance of benzene vapour.
Embodiment 8, get raw fiber 12.2 gram, with immersion in 200 milliliter of 6.25% BAS 10 hours, pull out, wring out, behind the low temperature drying, boric acid load capacity on raw fiber is 9wt%.Fiber after handling is positioned in the carbonization-activation stove, under the chlorine protection, is warming up to 800 ℃, reacted 90 minutes.Naturally cool then to room temperature, take out fiber and wash 120 ℃ of oven dry with water 5 times.The yield that records product is 32.9wt%, and more long-pending than table is 496 meters
2/ gram is to the 187 milligrams/gram of adsorbance of benzene vapour.
Claims (2)
1, a kind of technology of preparing activated carbon fibres by boric acid activating method; it is fully moistening to it is characterized in that placing boric acid aqueous solution to be dipped to fiber the cellulose fibre raw material; pull out and wring out; low temperature is dry down; the heating carbonization-activation is 20 to 120 minutes under nitrogen protection; the carbonization-activation temperature is 350 to 800 ℃, washes with water repeatedly after the cooling naturally then, 110 to 120 ℃ of oven dry.
2, a kind of technology of preparing activated carbon fibres by boric acid activating method as claimed in claim 1, the concentration that it is characterized in that boric acid aqueous solution is 2～15%.
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| CN99116239A CN1077926C (en) | 1999-06-11 | 1999-06-11 | Process for preparing activated carbon fibres by boric acid activating method |
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| CN99116239A CN1077926C (en) | 1999-06-11 | 1999-06-11 | Process for preparing activated carbon fibres by boric acid activating method |
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| CN1238395A true CN1238395A (en) | 1999-12-15 |
| CN1077926C CN1077926C (en) | 2002-01-16 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1102675C (en) * | 2000-10-11 | 2003-03-05 | 中国科学院山西煤炭化学研究所 | Air activating process for preparing activated carbon fibres |
| CN101864635A (en) * | 2010-05-25 | 2010-10-20 | 大连理工大学 | Method for manufacturing high-strength viscose-based active carbon fiber fabrics |
| CN103014921A (en) * | 2012-12-17 | 2013-04-03 | 中国科学院化学研究所 | Multi-hole carbon fiber and preparation method thereof |
| CN103225135A (en) * | 2013-05-09 | 2013-07-31 | 中国科学院化学研究所 | Porous carbon fiber, and preparation method and application thereof |
| CN103551115A (en) * | 2013-09-25 | 2014-02-05 | 蚌埠德美过滤技术有限公司 | Boric acid modified active carbon and preparation method thereof |
| CN110422843A (en) * | 2019-08-04 | 2019-11-08 | 大连理工大学 | A kind of environment-friendly preparation method thereof of the biomass-based active carbon material of nitrogen boron codope and its application |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB8422875D0 (en) * | 1984-09-11 | 1984-10-17 | Secr Defence | Fibrous activated carbon |
| GB8822518D0 (en) * | 1988-09-26 | 1988-11-02 | Cybertronics Ltd | Improvements in & relating to fibrous activated carbons |
| CN1031394C (en) * | 1990-06-13 | 1996-03-27 | 李孝忠 | Active carbon fibre mfg. method |
| CN1040866C (en) * | 1994-07-03 | 1998-11-25 | 中国科学院长春应用化学研究所 | Method for preparation of viscose fibre active carbon |
| CN1161306A (en) * | 1997-01-31 | 1997-10-08 | 山西丛林煤化有限公司 | Method for preparing active carbon |
| JPH1161573A (en) * | 1997-08-27 | 1999-03-05 | Oji Paper Co Ltd | Production of silicon carbide fiber |
-
1999
- 1999-06-11 CN CN99116239A patent/CN1077926C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1102675C (en) * | 2000-10-11 | 2003-03-05 | 中国科学院山西煤炭化学研究所 | Air activating process for preparing activated carbon fibres |
| CN101864635A (en) * | 2010-05-25 | 2010-10-20 | 大连理工大学 | Method for manufacturing high-strength viscose-based active carbon fiber fabrics |
| CN103014921A (en) * | 2012-12-17 | 2013-04-03 | 中国科学院化学研究所 | Multi-hole carbon fiber and preparation method thereof |
| CN103014921B (en) * | 2012-12-17 | 2014-09-17 | 中国科学院化学研究所 | Multi-hole carbon fiber and preparation method thereof |
| CN103225135A (en) * | 2013-05-09 | 2013-07-31 | 中国科学院化学研究所 | Porous carbon fiber, and preparation method and application thereof |
| CN103225135B (en) * | 2013-05-09 | 2015-12-23 | 中国科学院化学研究所 | Porous carbon fiber and preparation method thereof and application |
| CN103551115A (en) * | 2013-09-25 | 2014-02-05 | 蚌埠德美过滤技术有限公司 | Boric acid modified active carbon and preparation method thereof |
| CN110422843A (en) * | 2019-08-04 | 2019-11-08 | 大连理工大学 | A kind of environment-friendly preparation method thereof of the biomass-based active carbon material of nitrogen boron codope and its application |
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| CN1077926C (en) | 2002-01-16 |
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