CN1077926C - 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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- CN1077926C CN1077926C CN99116239A CN99116239A CN1077926C CN 1077926 C CN1077926 C CN 1077926C CN 99116239 A CN99116239 A CN 99116239A CN 99116239 A CN99116239 A CN 99116239A CN 1077926 C CN1077926 C CN 1077926C
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Abstract
The present invention relates to a method for preparing activated carbon fibers, which comprises: immersing the raw materials of cellulose fibers in boracic acids as carbonizing and activating agents; taking out the cellulose fibers to be dried and then putting the dried cellulose fibers in a heating furnace to be carbonized and activated for a certain time to obtain the activated carbon fiber. The method of the present invention has the advantages of convenient operation, high yield of products, low preparation cost and low impurity content.
Description
The present invention relates to the method that a kind of chemical activation prepares activated carbon fiber.
Activated carbon fiber has flourishing specific area 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 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: adopt chemical activation method; with boric acid is activator; 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 dry down, and next step heated carbonization-activation 20 to 120 minutes in nitrogen protection, and heating-up temperature is 350-800 ℃; naturally wash with water repeatedly after the cooling, 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 production costs, 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 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 the aperture-accumulation specific area relation curve of technology of the present invention at the activated carbon fiber of three kinds of different activation temperature preparations.
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, ordinate is accumulation specific surface (m
2/ g), abscissa is the aperture, 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. gets raw fiber 10.4 grams, soaks 24 hours with 200 milliliter of 2.5% BAS, pulls out, wrings out, and 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. gets raw fiber 8.0 grams, soaks 20 hours with 200 milliliter of 5% BAS, pulls out, wrings out, and 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 nitrogen 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. gets raw fiber 9.8 grams, soaks 2 hours with 200 milliliter of 7.5% BAS, pulls out, wrings out, and 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. gets raw fiber 11.4 grams, soaks 24 hours with 200 milliliter of 10% BAS, pulls out, wrings out, and 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. gets raw fiber 9.61 grams, soaks 10 hours with 200 milliliter of 12.5% BAS, pulls out, wrings out, and 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. gets raw fiber 8.88 grams, soaks 20 hours with 200 milliliter of 6.2% BAS, pulls out, wrings out, and 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. gets raw fiber 11.4 grams, soaks 15 hours with 200 milliliter of 6.2% BAS, pulls out, wrings out, and 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 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 specific area is 499 meters
2/ gram is to the 206 milligrams/gram of adsorbance of benzene vapour.
Embodiment 8. gets raw fiber 12.2 grams, soaks 10 hours with 200 milliliter of 6.25% BAS, pulls out, wrings out, and 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 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 specific area 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 characterized in that adopting chemical activation method; with boric acid is activator, and it is fully moistening to place boric acid aqueous solution to be dipped to fiber the cellulose fibre raw material, pulls out and wrings out; low temperature is dry down; the load capacity of boric acid on raw fiber is 9-90wt%, and next step heated carbonization-activation 20 to 120 minutes in nitrogen protection then, and heating-up temperature is 350-800 ℃; naturally wash with water repeatedly after the cooling, 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 is characterized in that the product yield reaches more than 30%.
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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 CN1238395A (en) | 1999-12-15 |
| CN1077926C true CN1077926C (en) | 2002-01-16 |
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Families Citing this family (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 |
| CN101864635B (en) * | 2010-05-25 | 2012-05-23 | 大连理工大学 | Method for manufacturing high-strength viscose-based active carbon fiber fabrics |
| 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 |
| 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 |
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 |
| US5202302A (en) * | 1988-09-26 | 1993-04-13 | Pena John M D De | Preparation of activated carbons by impregnation with a boron compound and a phosphorus compound |
| CN1114633A (en) * | 1994-07-03 | 1996-01-10 | 中国科学院长春应用化学研究所 | Method for preparation of viscose fibre active carbon |
| CN1031394C (en) * | 1990-06-13 | 1996-03-27 | 李孝忠 | Active carbon fibre mfg. method |
| 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 |
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1999
- 1999-06-11 CN CN99116239A patent/CN1077926C/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 |
| US5202302A (en) * | 1988-09-26 | 1993-04-13 | Pena John M D De | Preparation of activated carbons by impregnation with a boron compound and a phosphorus compound |
| CN1031394C (en) * | 1990-06-13 | 1996-03-27 | 李孝忠 | Active carbon fibre mfg. method |
| CN1114633A (en) * | 1994-07-03 | 1996-01-10 | 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 |
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