CN1068604A - The two steps of inner liner and hermetic type legal system is equipped with the technology of activated carbon fiber - Google Patents

The two steps of inner liner and hermetic type legal system is equipped with the technology of activated carbon fiber Download PDF

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CN1068604A
CN1068604A CN 92105859 CN92105859A CN1068604A CN 1068604 A CN1068604 A CN 1068604A CN 92105859 CN92105859 CN 92105859 CN 92105859 A CN92105859 A CN 92105859A CN 1068604 A CN1068604 A CN 1068604A
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minutes
high temperature
oven
activated carbon
carbon fiber
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CN1037623C (en
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符若文
陆来云
曾汉民
吕海峰
朱世平
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Sun Yat Sen University
National Sun Yat Sen University
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National Sun Yat Sen University
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Abstract

The present invention relates to a kind of activated carbon fiber preparation method.Take the method for inner bag sealing, the heating schedule according to predetermined is positioned over the inner bag that fibrous raw material is housed in the low temperature oven and high temperature furnace of constant temperature successively, obtains the activated carbon fiber of premium properties behind the carbonization-activation.The inventive method production equipment is simple, and is easy to operate, with short production cycle, the production efficiency height, and cost is low, and properties of product are good.

Description

The two steps of inner liner and hermetic type legal system is equipped with the technology of activated carbon fiber
The present invention relates to a kind of preparation method of activated carbon fiber.
Activated carbon fiber is a kind of new and effective sorbing material that early sixties grows up, compare with the sorbing material that activated carbon etc. is traditional, activated carbon fiber has specific area height, abundant, little, the even aperture distribution in aperture of micropore, architectural features such as a certain amount of surface functional group are arranged, thereby it has excellent absorption property to the organic matter in organic steam, inorganic gas, the aqueous solution, metal ion etc., not only adsorbance is big for it, adsorption rate is fast, crushing is little when the post method is adsorbed, suction phenomenon can not appear leaking, and desorption is easy, can repeatedly recycle.Particularly, activated carbon fiber also has special redox function, can with high volence metal ion former be metal simple-substance also, thereby integrate absorption, separate, reduce.Simultaneously, activated carbon fiber is high temperature resistant, acid and alkali-resistance, and anti-solvent can be made forms such as cloth, felt, paper, uses more flexible.Because the performance of activated carbon fiber excellence, it more and more widely is being applied to fields such as chemical industry, environmental protection, defence and military, electronics and the energy.
Activated carbon fiber manufacture method in the past can be divided into two kinds: first batch production technology, it two is continous mode production technologies.The batch process production process is: pretreated fibrillation is positioned in the stove, heats up gradually under inert gas shielding and carry out carbonization, feed the active gases activation, cooling naturally then treats to take out when furnace temperature drops to room temperature product.This process production equipment is simple, but programming rate is slow, and cooling rate is slower, and the production cycle is very long, and production efficiency is low, and energy consumption is big, the cost height; The continous mode production technology is to utilize transmission device that pretreated fiber is sent into reacting furnace continuously, fiber carries out obtaining product after carbonization and the activation through different humidity provinces continuously, though this technology can be enhanced productivity, production equipment is complicated, equipment investment is bigger, and technology controlling and process is difficult.
The objective of the invention is to study the technology that a kind of improved production activated carbon fiber is provided, overcome the shortcoming of prior art, reach and shorten the production cycle, enhance productivity, reduce energy consumption, the effect that reduces cost.
Method of the present invention is: with the manufacture process of activated carbon fiber be divided into two the stage-low temperature oven reaction and high temperature furnace react.Low temperature oven and high temperature furnace are distinguished constant temperature at a certain temperature; Be contained in the flue sealing, logical nitrogen protection through pretreated fibrous raw material; Be positioned over successively in low temperature oven and the high temperature furnace then and react certain hour, feed steam activation again; Reaction and activation finish, and flue is hung out cooling, and temperature drops to and (is generally and reduces to room temperature) the taking-up product below 100 ℃.
The temperature of low temperature oven is controlled at 200 to 500 ℃ of scopes in the inventive method, is generally 300~400 ℃; The high temperature furnace temperature is controlled at 800~950 ℃ of scopes.The reaction time of sample in low temperature oven was controlled at 20~60 minutes, was generally 30~40 minutes; Carbonization time in high temperature furnace 20~40 minutes, 40~90 minutes time of water flowing steam activation in high temperature furnace.
Flue of the present invention is generally made with stainless steel; preferably adopt the preheating of spiral air inlet pipe to strengthen protecting gas and to activate gas, and can increase temperature and atmosphere evenness, gas sprays into from the bottom; tail gas is discharged from flue top escape pipe, and flue top is incubated to increase heat preservation zone with insulation material.
Can supporting two to four high temperature furnaces of low temperature oven when method of the present invention is implemented, a plurality of flues are produced continuously, reach the effect of uninterrupted production activated carbon fiber, and production efficiency improves greatly.
When adopting the inventive method to make activated carbon fiber, the carbonization-activation time needs 120~140 minutes approximately, temperature fall time needs 40~60 minutes approximately, total production cycle only needs about 160 to 200 minutes, shorten approximately 2/3~1/2 than single stove batch production technology carbonization-activation time, total production cycle shortens about 12 times.And, because low temperature oven and high temperature furnace always are in temperature constant state in the technology of the present invention, avoided resembling intensification and temperature-fall period in the batch process, energy consumption significantly reduces.
The production equipment that the present invention uses is simple, and cost is low, and is easy to operate, and prepared activated carbon fiber yield can be controlled between 15~20wt%, and specific area can reach 900~1500 meters 2/ gram.This technology and equipment also can be produced multi-form active-carbon fibre materials such as activated carbon-fiber felt, cloth, paper.
The actual heating curve of flue when Fig. 1 and Fig. 2 are to use explained hereafter activated carbon fiber of the present invention.Wherein curve (1) is 200 ℃ of low temperature oven, and flue is placed the 40 minutes time (hereinafter to be referred as standing time) in the low temperature oven; Curve (2) is 300 ℃ of low temperature oven, 40 minutes standing times; Curve (3) is 500 ℃ of low temperature oven, 30 minutes standing times; 400 ℃ of curve (4) low temperature oven, 60 minutes standing times; 400 ℃ of curve (5) low temperature oven, 20 minutes standing times.The high temperature furnace temperature of curve (1) to (5) is 890 ℃.By regulating the design temperature and the reaction time of low temperature oven and high temperature furnace, controlled prepared material reacts by different heating schedules.Can control technical process is that staged heats up, and also can being controlled to be uniformly, continous mode heats up.
The actual natural temperature lowering curve of flue when Fig. 3 is to use explained hereafter activated carbon fiber of the present invention.General nature cooling 37 minutes, the flue temperature can drop to 170 ℃.
The invention will be further described by the following examples:
Embodiment 1 gets raw fiber 237 grams, soaks with 5% diammonium hydrogen phosphate, behind the filtering drying, be positioned in the flue, and sealing, logical nitrogen protection is positioned over reaction and activation in low temperature oven and the high temperature furnace successively.Temperature of low-oven is 200 ℃, and the high temperature furnace temperature is 890 ℃, and the reaction time in low temperature oven is 40 minutes, and in the 30 minutes reaction time in the high temperature furnace, then water flowing steam activates 60 fens, 890 ℃ of activation temperatures in high temperature furnace.Reaction finishes, and hangs out flue, is cooled to room temperature naturally, takes out product, and the yield that records product is 16.9wt%, and more long-pending than table is 859 meters 2/ gram is respectively 378 and 701 milligrams/gram to the adsorbance of benzene and carbon tetrachloride.
Embodiment 2 gets raw fiber 234 grams, soaks with 5% diammonium hydrogen phosphate, behind the filtering drying, be positioned in the flue, and sealing, logical nitrogen protection is positioned over reaction and activation in low temperature oven and the high temperature furnace successively.Temperature of low-oven is 500 ℃, and the high temperature furnace temperature is 890 ℃, and the reaction time in low temperature oven is 30 minutes, and the reaction time is 30 minutes in the high temperature furnace, and then water flowing steam activates 60 fens, 890 ℃ of activation temperatures in high temperature furnace.Reaction finishes, and hangs out flue, is cooled to room temperature naturally, takes out product, and the yield that records product is 24.8%wt%, and specific area is 670 meters 2/ gram is respectively 361 and 672 milligrams/gram to the adsorbance of benzene and carbon tetrachloride.
Embodiment 3 gets raw fiber 224 grams, soaks with 5% diammonium hydrogen phosphate, behind the filtering drying, be positioned in the flue, and sealing, logical nitrogen protection is positioned over reaction and activation in low temperature oven and the high temperature furnace successively.Temperature of low-oven is 400 ℃, and the high temperature furnace temperature is 890 ℃, and the reaction time in low temperature oven is 20 minutes, and the reaction time is 30 minutes in the high temperature furnace, and then water flowing steam activates 60 fens, 890 ℃ of activation temperatures in high temperature furnace.Reaction finishes, and hangs out flue, is cooled to room temperature naturally, takes out product, and the yield that records product is 18.5wt%, and specific area is 1017 meters 2/ gram is 742 a milligrams/gram to the adsorbance of carbon tetrachloride.
Embodiment 4 gets raw fiber 234 grams, soaks with 5% diammonium hydrogen phosphate, behind the filtering drying, be positioned in the flue, and sealing, logical nitrogen protection is positioned over reaction and activation in low temperature oven and the high temperature furnace successively.Temperature of low-oven is 400 ℃, and the high temperature furnace temperature is 890 ℃, and the reaction time in low temperature oven is 60 minutes, and the reaction time is 30 minutes in the high temperature furnace, and then water flowing steam activates 60 fens, 890 ℃ of activation temperatures in high temperature furnace.Reaction finishes, and hangs out flue, is cooled to room temperature naturally, takes out product, and the yield that records product is 18.6wt%, and specific area is 912 meters 2/ gram is 584 a milligrams/gram to the adsorbance of carbon tetrachloride.
Embodiment 5 gets raw fiber 233 grams, soaks with 5% diammonium hydrogen phosphate, behind the filtering drying, be positioned in the flue, and sealing, logical nitrogen protection is positioned over reaction and activation in low temperature oven and the high temperature furnace successively.Temperature of low-oven is 400 ℃, and the high temperature furnace temperature is 700 ℃, and the reaction time in low temperature oven is 40 minutes, and the reaction time is 30 minutes in the high temperature furnace, and then water flowing steam activates 60 fens in high temperature furnace, and activation temperature is 890 ℃.Reaction finishes, and hangs out flue, is cooled to room temperature naturally, takes out product, and the yield that records product is 15.2wt%, and specific area is 648 meters 2/ gram is 334 a milligrams/gram to the adsorbance of benzene.
Embodiment 6 gets raw fiber 234 grams, soaks with 5% diammonium hydrogen phosphate, behind the filtering drying, be positioned in the flue, and sealing, logical nitrogen protection is positioned over reaction and activation in low temperature oven and the high temperature furnace successively.Temperature of low-oven is 400 ℃, and the high temperature furnace temperature is 920 ℃, and the reaction time in low temperature oven is 40 minutes, and the reaction time is 30 minutes in the high temperature furnace, and then water flowing steam activates 60 fens, 920 ℃ of activation temperatures in high temperature furnace.Reaction finishes, and hangs out flue, is cooled to room temperature naturally, takes out product, and the yield that records product is 13.4wt%, and specific area is 980 meters 2/ gram is respectively 525 and 1000 milligrams/gram to the adsorbance of benzene and carbon tetrachloride.
Embodiment 7 gets raw fiber 230 grams, soaks with 5% diammonium hydrogen phosphate, behind the filtering drying, be positioned in the flue, and sealing, logical nitrogen protection is positioned over reaction and activation in low temperature oven and the high temperature furnace successively.Temperature of low-oven is 400 ℃, and the high temperature furnace temperature is 890 ℃, and the reaction time in low temperature oven is 40 minutes, and in the 0 minute reaction time in the high temperature furnace, then water flowing steam activates 90 fens, 890 ℃ of activation temperatures in high temperature furnace.Reaction finishes, and hangs out flue, is cooled to room temperature naturally, takes out product, and the yield that records product is 19.1wt%, and specific area is 860 meters 2/ gram is respectively 455 and 1090 milligrams/gram to the adsorbance of benzene and carbon tetrachloride.

Claims (5)

1, a kind of method for preparing activated carbon fiber is characterized in that and will be contained in the flue through pretreated fibrous raw material, sealing, logical nitrogen protection, put into low temperature oven and reacted 20~60 minutes, move into again and react (carbonization) 20~40 minutes in the high temperature furnace, fed steam activation then 40~90 minutes; Temperature of low-oven is 200~500 ℃, and the high temperature furnace temperature is 800~950 ℃; Reaction and activation finish, and flue is hung out, and product is taken out in the cooling back.
2, in accordance with the method for claim 1, it is characterized in that temperature of low-oven is 300~400 ℃.
3,, it is characterized in that the time of reacting is 30~40 minutes in low temperature oven according to claim 1 or 2 described methods.
4, in accordance with the method for claim 1, it is characterized in that reaction (carbonization) time is 30 minutes in high temperature furnace.
5,, it is characterized in that the time of water flowing steam activation in high temperature furnace is 60 minutes according to claim 1 or 4 described methods.
CN92105859A 1992-07-17 1992-07-17 Active carbon fibre preparing process by two steps of inner liner and hermetic type Expired - Fee Related CN1037623C (en)

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CN92105859A CN1037623C (en) 1992-07-17 1992-07-17 Active carbon fibre preparing process by two steps of inner liner and hermetic type

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CN1037623C CN1037623C (en) 1998-03-04

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102140710A (en) * 2011-02-28 2011-08-03 江苏科净炭纤维有限公司 Preparation process of low-wind-resistant activated carbon fiber
CN102817112A (en) * 2012-09-11 2012-12-12 长春高琦聚酰亚胺材料有限公司 Preparation method of activated carbon fibers
CN103205825A (en) * 2013-04-24 2013-07-17 湖北中烟工业有限责任公司 Method for preparing cigarette filamentary carbon heat source material by ethanol

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1246374A (en) * 1983-10-24 1988-12-13 Steve Rowland Two stage high consistency refiner

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102140710A (en) * 2011-02-28 2011-08-03 江苏科净炭纤维有限公司 Preparation process of low-wind-resistant activated carbon fiber
CN102817112A (en) * 2012-09-11 2012-12-12 长春高琦聚酰亚胺材料有限公司 Preparation method of activated carbon fibers
CN102817112B (en) * 2012-09-11 2014-10-15 长春高琦聚酰亚胺材料有限公司 Preparation method of activated carbon fibers
CN103205825A (en) * 2013-04-24 2013-07-17 湖北中烟工业有限责任公司 Method for preparing cigarette filamentary carbon heat source material by ethanol
CN103205825B (en) * 2013-04-24 2014-10-08 湖北中烟工业有限责任公司 Method for preparing cigarette filamentary carbon heat source material by ethanol

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