CN103272562B - 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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- CN103272562B CN103272562B CN201310243243.3A CN201310243243A CN103272562B CN 103272562 B CN103272562 B CN 103272562B CN 201310243243 A CN201310243243 A CN 201310243243A CN 103272562 B CN103272562 B CN 103272562B
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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 active carbon and prepare sorbing material field, be specifically related to a kind of preparation method of filtrate based active carbon fiber.
Background technology
NACF (Activated Carbon Fiber, ACF) grows up on Industry of Carbon Fiber basis, is the third generation product after powdery, granular active carbon.As the new and effective sorbing material of one, it has, and specific area is large, micropore enriches, little and the narrowly distributing in aperture, adsorbance is large, adsorption rate is fast, and high adsorption capacity, easily regenerates, technological flexibility large (can be made into the variforms such as yarn, cloth, felt, paper), is widely used in the aspects such as chemical industry, environmental protection, catalysis, medical, food hygiene.Due to 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.The organic fiber being used as at present ACF presoma mainly contains viscose base, polyacrylonitrile-radical, phenolic aldehyde base and asphaltic base, and all realizes industrialization, but the ACF preparing gained like this to there is cost higher, easy contaminated environment simultaneously.
China is coal-fired big country, and burning of coal will discharge a large amount of pollutants (toxic gas and dust).What current China was used for controlling coal fired thermal power plant burning and exhausting soot dust granule is take filtrate as the sack cleaner of core, and due to long high-temperature operation, these filtrates will lose the effect of dedusting gradually, thus become trade waste.And filtrate is substantially by fibrous, and the feasibility preparing NACF is very high, can also greatly reduce costs.Therefore, making full use of these filtrate discarded objects for otherwise purposes is a good thinking.Through retrieval, also do not find about being the open report that carbon source prepares NACF with needle punched filter material discarded object at present.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of filtrate based active carbon fiber, the method cost is low, and feasibility is high, can reach the effect of resource reutilization, simultaneously for the process of trade waste provides a good thinking.
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for filtrate based active carbon fiber, with discarded Nomex fiber for carbon source, through carbonization, the NACF that KOH chemical activation is obtained.Comprise the steps:
(1) filtrate that given up by Nomex is cut into small pieces, and uses H
2the mixed solution ultrasonic immersing 20-30 min of O and ethanol, more repeatedly clean 3 ~ 4 times by deionized water, be placed in vacuum drying chamber 80-110 DEG C and dry 12-24 h;
(2) filtrate that step (1) is dry is heated to 700-900 DEG C with certain heating rate under inert gas shielding, carries out carbonization treatment, be cooled to room temperature;
(3) product after carbonization is fully ground, cross 80-100 mesh sieve, then fully mix with KOH powder, be finally heated to 700-900 DEG C of activation process with certain heating rate under an inert gas, be cooled to room temperature;
(4) after the product after activation being flooded 12-24 h with hydrochloric acid solution, more repeatedly clean 3-4 time by deionized water, to remove remaining activator, then 80-110 DEG C of dry 12-24h in vacuum drying chamber, namely obtains filtrate based active carbon fiber.
Step (2) and the heating rate described in (3) are 10 DEG C/min.
Step (2) and the inert gas described in (3) are nitrogen or argon gas.
The mass ratio of the carbide described in step (3) and KOH is 1 ~ 4:1.
Carbonization time described in step (2) is 1-2h.
Soak time described in step (3) is 30-120 min.
Concentration of hydrochloric acid solution described in step (4) is 1 ~ 10wt%.
NACF obtained by the present invention utilizes industrial Nomex waste material after carbonization, prepares under the activation of KOH.KOH take part in the priming reaction of carbon, the K that reaction produces
2o at high temperature can with the H of reproducibility
2generate simple substance potassium with C reaction, potassium (boiling point 726 DEG C) can produce potassium steam more than 800 DEG C, and gets between carbon-coating, plays activation mutually, thus obtain the NACF of high-carbon yield and high-specific surface area to crystallite.
Compared with prior art, beneficial effect of the present invention is:
(1) raw material is easy to get, and cost is low, is 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 the aspects such as environmental protection, chemical industry, medical and catalysis, has wide practical use;
(4) the preparation thinking of products obtained therefrom is that the process of trade waste provides a good thinking, is conducive to the protection of environment.
Accompanying drawing explanation
Fig. 1 is the XRD diffracting spectrum of the obtained filtrate base carbon fibre of embodiment 1 and NACF.
Fig. 2 is the stereoscan photograph of the filtrate based active carbon fiber that embodiment 1 obtains.
Detailed description of the invention
Embodiment 1
(1) filtrate that given up by Nomex is cut into small pieces, and uses H
2the mixed solution ultrasonic immersing 20-30 min of O and ethanol, more repeatedly clean 3 ~ 4 times by deionized water, is then placed in vacuum drying chamber 80-110 DEG C by the filtrate after cleaned and dries 12-24 h;
(2) by filtrate dry in (1) at inert gas (N
2) be heated to 750 DEG C with the heating rate of 10 DEG C/min under protection, carry out carbonization treatment 1 h, be cooled to room temperature;
(3) fully ground by the product after carbonization, sieve 80-100 order, then fully mixes with KOH powder, finally at inert gas (N according to certain mass ratio (1:1)
2) under be heated to 750 DEG C with the heating rate of 10 DEG C/min, and activation process 120 min, be cooled to room temperature;
(4) after the product after activation being flooded 12-24 h with the hydrochloric acid solution of certain mass concentration, repeatedly clean 3-4 time by deionized water again, to remove remaining activator, then 80-110 DEG C of dry 12-24 h in vacuum drying chamber, can obtain filtrate based active carbon fiber.
Fig. 1 is the XRD collection of illustrative plates of the present embodiment gained.From collection of illustrative plates, we can show that filtrate is all carbonized as graphite, and after activation, stone degree of graphitization decreases.
Fig. 2 is the SEM collection of illustrative plates of the present embodiment gained.Can find out that from collection of illustrative plates obtained NACF surface has micropore to exist, and it is relatively uniform to distribute.
Embodiment 2
(1) filtrate that given up by Nomex is cut into small pieces, and uses H
2the mixed solution ultrasonic immersing 20-30 min of O and ethanol, more repeatedly clean 3 ~ 4 times by deionized water, is then placed in vacuum drying chamber 80-110 DEG C by the filtrate after cleaned and dries 12-24 h;
(2) by filtrate dry in (1) at inert gas (N
2) be heated to 800 DEG C with the heating rate of 10 DEG C/min under protection, carry out carbonization treatment 1 h, be cooled to room temperature;
(3) fully ground by the product after carbonization, sieve 80-100 order, then fully mixes with KOH powder, finally at inert gas (N according to certain mass ratio (1:2)
2) under be heated to 800 DEG C with the heating rate of 10 DEG C/min, and activation process 90 min, be cooled to room temperature.
(4) after the product after activation being flooded 12-24 h with the hydrochloric acid solution of certain mass concentration, repeatedly clean 3-4 time by deionized water again, to remove remaining activator, then 80-110 DEG C of dry 12-24 h in vacuum drying chamber, can obtain filtrate based active carbon fiber.
Embodiment 3
(1) filtrate that given up by Nomex is cut into small pieces, and uses H
2the mixed solution ultrasonic immersing 20-30 min of O and ethanol, more repeatedly clean 3 ~ 4 times by deionized water, is then placed in vacuum drying chamber 80-110 DEG C by the filtrate after cleaned and dries 12-24 h;
(2) by filtrate dry in (1) at inert gas (N
2) be heated to 850 DEG C with the heating rate of 10 DEG C/min under protection, carry out carbonization treatment 2 h, be cooled to room temperature;
(3) fully ground by the product after carbonization, sieve 80-100 order, then fully mixes with KOH powder, finally at inert gas (N according to certain mass ratio (1:3)
2) under be heated to 850 DEG C with the heating rate of 10 DEG C/min, and activation process 60 min, be cooled to room temperature.
(4) after the product after activation being flooded 12-24 h with the hydrochloric acid solution of certain mass concentration, repeatedly clean 3-4 time by deionized water again, to remove remaining activator, then 80-110 DEG C of dry 12-24 h in vacuum drying chamber, can obtain filtrate based active carbon fiber.
Embodiment 4
(1) filtrate that given up by Nomex is cut into small pieces, and uses H
2the mixed solution ultrasonic immersing 20-30 min of O and ethanol, more repeatedly clean 3 ~ 4 times by deionized water, is then placed in vacuum drying chamber 80-110 DEG C by the filtrate after cleaned and dries 12-24 h;
(2) by filtrate dry in (1) at inert gas (N
2) be heated to 900 DEG C with the heating rate of 10 DEG C/min under protection, carry out carbonization treatment 2 h, be cooled to room temperature;
(3) fully ground by the product after carbonization, sieve 80-100 order, then fully mixes with KOH powder, finally at inert gas (N according to certain mass ratio (1:4)
2) under be heated to 900 DEG C with the heating rate of 10 DEG C/min, and activation process 30 min, be cooled to room temperature.
(4) after the product after activation being flooded 12-24 h with the hydrochloric acid solution of certain mass concentration, repeatedly clean 3-4 time by deionized water again, to remove remaining activator, then 80-110 DEG C of dry 12-24 h in vacuum drying chamber, can obtain filtrate based active carbon fiber.
Table 1 is the NACF specific surface performance parameter of the present embodiment gained
The specific area of NACF obtained is as can be seen from the table up to 1685 m
2/ g, and aperture integrated distribution is at about 2 nm.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (1)
1. a preparation method for filtrate based active carbon fiber, is characterized in that: with discarded Nomex fiber for carbon source, through carbonization, the NACF that KOH chemical activation is obtained;
Comprise the steps:
(1) filtrate that given up by Nomex is cut into small pieces, and uses H
2the mixed solution ultrasonic immersing 20-30 min of O and ethanol, more repeatedly clean 3 ~ 4 times by deionized water, be placed in vacuum drying chamber 80-110 DEG C and dry 12-24 h;
(2) filtrate that step (1) is dry is heated to 700-900 DEG C with certain heating rate under inert gas shielding, carries out carbonization treatment, be cooled to room temperature;
(3) product after carbonization is fully ground, cross 80-100 mesh sieve, then fully mix with KOH powder, be finally heated to 700-900 DEG C of activation process with certain heating rate under an inert gas, be cooled to room temperature;
(4) after the product after activation being flooded 12-24 h with hydrochloric acid solution, more repeatedly clean 3-4 time by deionized water, to remove remaining activator, then 80-110 DEG C of dry 12-24h in vacuum drying chamber, namely obtains filtrate based active carbon fiber;
Step (2) and the heating rate described in (3) are 10 DEG C/min;
Step (2) and the inert gas described in (3) are nitrogen or argon gas;
Product after carbonization described in step (3) and the mass ratio of KOH are 1 ~ 4:1;
The time of the carbonization treatment described in step (2) is 1-2h;
The time of the activation process described in step (3) is 30-120 min;
Concentration of hydrochloric acid solution described in step (4) is 1 ~ 10wt%.
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| CN104001371A (en) * | 2014-05-30 | 2014-08-27 | 福州大学 | Method for recycling waste dust removal filter material |
| 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 |
| CN104437375B (en) * | 2014-11-27 | 2017-05-10 | 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 |
| CN112981708B (en) * | 2021-05-11 | 2021-08-17 | 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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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| 宫传东.废旧有机纤维制备活性炭纤维(ACF)的工艺研究.《中国优秀硕士学位论文全文数据库 工程技术I辑》.2008,(第12期),第27页第4段,第28页"4.2.1 炭化"和"4.2.3 KOH活化法". * |
| 针刺毡滤料的优势及应用前景;孙志钜;《产业用纺织品》;20091231(第12期);第38-41页 * |
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