CN103272562A - Preparation method of filter material base activated carbon fiber - Google Patents
Preparation method of filter material base activated carbon fiber Download PDFInfo
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- CN103272562A CN103272562A CN2013102432433A CN201310243243A CN103272562A CN 103272562 A CN103272562 A CN 103272562A CN 2013102432433 A CN2013102432433 A CN 2013102432433A CN 201310243243 A CN201310243243 A CN 201310243243A CN 103272562 A CN103272562 A CN 103272562A
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Abstract
The invention discloses a preparation method of filter material base activated carbon fiber, which takes waste punched felt fiber as a carbon source to prepare the activated carbon fiber through carbonization and KOH chemical activation. The method is low in cost, has high feasibility, can achieve an effect of resource reuse, and simultaneously provides ideal thought for the industrial waste disposal.
Description
Technical field
The invention belongs to resource reutilization Preparation of Activated Carbon sorbing material field, be specifically related to a kind of preparation method of filtrate based active carbon fiber.
Background technology
(Activated Carbon Fiber's NACF ACF) grows up at the carbon fiber industrial foundation, is the third generation product after powdery, granular active carbon.As a kind of new and effective sorbing material, it has, and specific area is big, micropore abundant, little and the narrowly distributing in aperture, adsorbance is big, adsorption rate is fast, high adsorption capacity, easily regeneration, technological flexibility big (can be made into variforms such as yarn, cloth, felt, paper) is widely used in aspects such as chemical industry, environmental protection, catalysis, medical, food hygiene.Because the difference of precursor material, the production of ACF also can be different, in general, adopts different treatment process can produce different pore structures and absorption property.At present the organic fiber as the ACF presoma mainly contains viscose base, polyacrylonitrile-radical, phenolic aldehyde base and asphaltic base, and has all realized industrialization, but the ACF for preparing gained like this exists cost higher, simultaneously contaminated environment easily.
China is coal-fired big country, and burning of coal will be discharged a large amount of pollutant (toxic gas and dust).What at present China was used for controlling coal fired thermal power plant burning and exhausting soot dust granule is to be the sack cleaner of core with the filtrate, because high-temperature operation for a long time, these filtrates will lose the effect of dedusting gradually, thereby become trade waste.And filtrate is substantially by fibrous, and the feasibility of preparation NACF is very high, can also reduce cost greatly.Therefore, taking full advantage of these filtrate discarded objects is a good idea for otherwise purposes.By retrieval, also do not find at present about being the open report that carbon source prepares NACF with the needle punched filter material discarded object.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of filtrate based active carbon fiber, this method cost is low, and the feasibility height can reach the effect of resource reutilization, and the processing for trade waste simultaneously provides a good idea.
For achieving the above object, the present invention adopts following technical scheme:
A kind of preparation method of filtrate based active carbon fiber is carbon source with discarded Nomex fiber, through carbonization, and the NACF that the KOH chemical activation makes.Comprise the steps:
(1) the useless filtrate of Nomex is cut into small pieces, uses H
2The mixed solution ultrasonic immersing 20-30 min of O and ethanol cleans 3 ~ 4 times repeatedly with deionized water again, places vacuum drying chamber 80-110 ℃ of baking 12-24 h;
(2) step (1) is dry filtrate is heated to 700-900 ℃ with certain heating rate under inert gas shielding, carry out carbonization treatment, is cooled to room temperature;
(3) product after the carbonization is fully ground, cross the 80-100 mesh sieve, fully mix with the KOH powder then, under inert gas, be heated to 700-900 ℃ of activation processing with certain heating rate at last, be cooled to room temperature;
(4) product after will activating with hydrochloric acid solution dipping 12-24 h after, clean 3-4 time repeatedly with deionized water again, to remove remaining activator, 80-110 ℃ of dry 12-24h in vacuum drying chamber namely obtains the filtrate based active carbon fiber then.
Heating rate described in step (2) and (3) is 10 ℃/min.
Inert gas described in step (2) and (3) is nitrogen or argon gas.
The mass ratio of carbide described in the step (3) and KOH is 1 ~ 4:1.
Carbonization time described in the step (2) is 1-2h.
Soak time described in the step (3) is 30-120 min.
Concentration of hydrochloric acid solution described in the step (4) is 1 ~ 10wt%.
The prepared NACF of the present invention is to utilize industrial Nomex waste material after carbonization, prepares under the activation of KOH.KOH has participated in the priming reaction of carbon, the K that reaction produces
2O at high temperature can with the H of reproducibility
2Reaction generates simple substance potassium with C, and potassium (726 ℃ of boiling points) can produce potassium steam more than 800 ℃, and gets between carbon-coating, crystallite is played activation mutually, thereby obtain the NACF of high-carbon yield and high-specific surface area.
Compared with prior art, beneficial effect of the present invention is:
(1) raw material is easy to get, and cost is low, is the industrial waste gas filtrate, is conducive to industrialized production;
(2) raw material fibre-bearing amount is very high, preparation method's technology maturation;
(3) products obtained therefrom ACF can be used for aspects such as environmental protection, chemical industry, medical and catalysis, has wide practical use;
(4) the preparation thinking of products obtained therefrom is conducive to the protection of environment for the processing of trade waste provides a good idea.
Description of drawings
Fig. 1 is the filtrate base carbon fibre that makes of embodiment 1 and the XRD diffracting spectrum of NACF.
Fig. 2 is the stereoscan photograph of the filtrate based active carbon fiber that makes of embodiment 1.
The specific embodiment
Embodiment 1
(1) the useless filtrate of Nomex is cut into small pieces, uses H
2The mixed solution ultrasonic immersing 20-30 min of O and ethanol cleans 3 ~ 4 times repeatedly with deionized water again, will clean filtrate later then and place vacuum drying chamber 80-110 ℃ of baking 12-24 h;
(2) with filtrate dry in (1) at inert gas (N
2) protect following heating rate with 10 ℃/min to be heated to 750 ℃, carry out carbonization treatment 1 h, be cooled to room temperature;
(3) product after the carbonization is fully ground, the 80-100 order that sieves fully mixes according to certain quality ratio (1:1) and KOH powder, then at last at inert gas (N
2) under be heated to 750 ℃ with the heating rate of 10 ℃/min, and activation processing 120 min are cooled to room temperature;
(4) behind the hydrochloric acid solution dipping 12-24 h of the product after will activating with certain mass concentration, clean 3-4 time repeatedly with deionized water again, to remove remaining activator, 80-110 ℃ of dry 12-24 h in vacuum drying chamber can obtain the filtrate based active carbon fiber then.
Fig. 1 is the XRD collection of illustrative plates of present embodiment gained.We can draw filtrate and all are carbonized and are graphite from collection of illustrative plates, and activation back stone degree of graphitization decreases.
Fig. 2 is the SEM collection of illustrative plates of present embodiment gained.The NACF surface that makes as can be seen from collection of illustrative plates has micropore to exist, and it is even relatively to distribute.
(1) the useless filtrate of Nomex is cut into small pieces, uses H
2The mixed solution ultrasonic immersing 20-30 min of O and ethanol cleans 3 ~ 4 times repeatedly with deionized water again, will clean filtrate later then and place vacuum drying chamber 80-110 ℃ of baking 12-24 h;
(2) with filtrate dry in (1) at inert gas (N
2) protect following heating rate with 10 ℃/min to be heated to 800 ℃, carry out carbonization treatment 1 h, be cooled to room temperature;
(3) product after the carbonization is fully ground, the 80-100 order that sieves fully mixes according to certain quality ratio (1:2) and KOH powder, then at last at inert gas (N
2) under be heated to 800 ℃ with the heating rate of 10 ℃/min, and activation processing 90 min are cooled to room temperature.
(4) behind the hydrochloric acid solution dipping 12-24 h of the product after will activating with certain mass concentration, clean 3-4 time repeatedly with deionized water again, to remove remaining activator, 80-110 ℃ of dry 12-24 h in vacuum drying chamber can obtain the filtrate based active carbon fiber then.
Embodiment 3
(1) the useless filtrate of Nomex is cut into small pieces, uses H
2The mixed solution ultrasonic immersing 20-30 min of O and ethanol cleans 3 ~ 4 times repeatedly with deionized water again, will clean filtrate later then and place vacuum drying chamber 80-110 ℃ of baking 12-24 h;
(2) with filtrate dry in (1) at inert gas (N
2) protect following heating rate with 10 ℃/min to be heated to 850 ℃, carry out carbonization treatment 2 h, be cooled to room temperature;
(3) product after the carbonization is fully ground, the 80-100 order that sieves fully mixes according to certain quality ratio (1:3) and KOH powder, then at last at inert gas (N
2) under be heated to 850 ℃ with the heating rate of 10 ℃/min, and activation processing 60 min are cooled to room temperature.
(4) behind the hydrochloric acid solution dipping 12-24 h of the product after will activating with certain mass concentration, clean 3-4 time repeatedly with deionized water again, to remove remaining activator, 80-110 ℃ of dry 12-24 h in vacuum drying chamber can obtain the filtrate based active carbon fiber then.
Embodiment 4
(1) the useless filtrate of Nomex is cut into small pieces, uses H
2The mixed solution ultrasonic immersing 20-30 min of O and ethanol cleans 3 ~ 4 times repeatedly with deionized water again, will clean filtrate later then and place vacuum drying chamber 80-110 ℃ of baking 12-24 h;
(2) with filtrate dry in (1) at inert gas (N
2) protect following heating rate with 10 ℃/min to be heated to 900 ℃, carry out carbonization treatment 2 h, be cooled to room temperature;
(3) product after the carbonization is fully ground, the 80-100 order that sieves fully mixes according to certain quality ratio (1:4) and KOH powder, then at last at inert gas (N
2) under be heated to 900 ℃ with the heating rate of 10 ℃/min, and activation processing 30 min are cooled to room temperature.
(4) behind the hydrochloric acid solution dipping 12-24 h of the product after will activating with certain mass concentration, clean 3-4 time repeatedly with deionized water again, to remove remaining activator, 80-110 ℃ of dry 12-24 h in vacuum drying chamber can obtain the filtrate based active carbon fiber then.
Table 1 is the NACF specific surface performance parameter of present embodiment gained
The specific area of the NACF that makes as can be seen from the table is up to 1685 m
2/ g, and the aperture is concentrated and to be distributed in about 2 nm.
The above only is preferred embodiment of the present invention, and all equalizations of doing according to the present patent application claim change and modify, and all should belong to covering scope of the present invention.
Claims (8)
1. the preparation method of a filtrate based active carbon fiber is characterized in that: be carbon source with discarded Nomex fiber, and through carbonization, the NACF that the KOH chemical activation makes.
2. the preparation method of filtrate based active carbon fiber according to claim 1 is characterized in that: comprise the steps:
(1) the useless filtrate of Nomex is cut into small pieces, uses H
2The mixed solution ultrasonic immersing 20-30 min of O and ethanol cleans 3 ~ 4 times repeatedly with deionized water again, places vacuum drying chamber 80-110 ℃ of baking 12-24 h;
(2) step (1) is dry filtrate is heated to 700-900 ℃ with certain heating rate under inert gas shielding, carry out carbonization treatment, is cooled to room temperature;
(3) product after the carbonization is fully ground, cross the 80-100 mesh sieve, fully mix with the KOH powder then, under inert gas, be heated to 700-900 ℃ of activation processing with certain heating rate at last, be cooled to room temperature;
(4) product after will activating with hydrochloric acid solution dipping 12-24 h after, clean 3-4 time repeatedly with deionized water again, to remove remaining activator, 80-110 ℃ of dry 12-24h in vacuum drying chamber namely obtains the filtrate based active carbon fiber then.
3. the preparation method of filtrate based active carbon fiber according to claim 2, it is characterized in that: the heating rate described in step (2) and (3) is 10 ℃/min.
4. the preparation method of filtrate based active carbon fiber according to claim 2, it is characterized in that: the inert gas described in step (2) and (3) is nitrogen or argon gas.
5. the preparation method of filtrate based active carbon fiber according to claim 2, it is characterized in that: the mass ratio of the carbide described in the step (3) and KOH is 1 ~ 4:1.
6. the preparation method of filtrate based active carbon fiber according to claim 2, it is characterized in that: the carbonization time described in the step (2) is 1-2h.
7. the preparation method of filtrate based active carbon fiber according to claim 2, it is characterized in that: the soak time described in the step (3) is 30-120 min.
8. the preparation method of filtrate based active carbon fiber according to claim 2, it is characterized in that: the concentration of hydrochloric acid solution described in the step (4) is 1 ~ 10wt%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104001371A (en) * | 2014-05-30 | 2014-08-27 | 福州大学 | Method for recycling waste dust removal filter material |
| CN104307470A (en) * | 2014-09-30 | 2015-01-28 | 天津理工大学 | Preparation method of cellulose fiber-based active carbon fibers with high adsorption capacity as well as product and application of cellulose fiber-based active carbon fibers with high adsorption capacity |
| CN104437375A (en) * | 2014-11-27 | 2015-03-25 | 深圳市建筑科学研究院股份有限公司 | Preparation method of adsorbent material as well as analytical method |
| CN106564899A (en) * | 2016-11-08 | 2017-04-19 | 西安工程大学 | Method for preparing titanium dioxide/active carbon electrode material from waste cotton textiles |
| CN109570210A (en) * | 2018-10-23 | 2019-04-05 | 王汉之 | A method of soil metallic pollution is administered using nano-porous materials |
| CN112981708A (en) * | 2021-05-11 | 2021-06-18 | 宁波霓科新材料有限公司 | Degradable hybrid fiber breathable felt, preparation method and drying method thereof |
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| US2390780A (en) * | 1943-10-02 | 1945-12-11 | Sylvania Ind Corp | Process of making coated textile materials and the articles produced therefrom |
| CN102140709A (en) * | 2011-01-27 | 2011-08-03 | 济南大学 | Microporous activated carbon fiber and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104001371A (en) * | 2014-05-30 | 2014-08-27 | 福州大学 | Method for recycling waste dust removal filter material |
| CN104307470A (en) * | 2014-09-30 | 2015-01-28 | 天津理工大学 | Preparation method of cellulose fiber-based active carbon fibers with high adsorption capacity as well as product and application of cellulose fiber-based active carbon fibers with high adsorption capacity |
| CN104307470B (en) * | 2014-09-30 | 2016-06-29 | 天津理工大学 | Preparation method of cellulose fibre based active carbon fiber of a kind of high adsorption capacity and products thereof and application |
| CN104437375A (en) * | 2014-11-27 | 2015-03-25 | 深圳市建筑科学研究院股份有限公司 | Preparation method of adsorbent material as well as analytical method |
| CN106564899A (en) * | 2016-11-08 | 2017-04-19 | 西安工程大学 | Method for preparing titanium dioxide/active carbon electrode material from waste cotton textiles |
| CN109570210A (en) * | 2018-10-23 | 2019-04-05 | 王汉之 | A method of soil metallic pollution is administered using nano-porous materials |
| CN112981708A (en) * | 2021-05-11 | 2021-06-18 | 宁波霓科新材料有限公司 | Degradable hybrid fiber breathable felt, preparation method and drying method thereof |
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