CN106006638A - Preparation method of high-penetration microporous granular active carbon - Google Patents
Preparation method of high-penetration microporous granular active carbon Download PDFInfo
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- CN106006638A CN106006638A CN201610351083.8A CN201610351083A CN106006638A CN 106006638 A CN106006638 A CN 106006638A CN 201610351083 A CN201610351083 A CN 201610351083A CN 106006638 A CN106006638 A CN 106006638A
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- activated carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
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Abstract
The invention relates to a preparation method of high-penetration microporous granular active carbon, belonging to the technical field of waste recycling or reprocessing. The preparation method comprises the following steps: treating waste wool fiber with a sulfuric acid solution; performing acid rolling, baking carbonization and impurity removal; neutralizing and adding a nonionic detergent to remove fat; finally, cleaning and drying to obtain clean wool fiber; and pre-carbonizing and activating the clean wool fiber to obtain active carbon fiber. The preparation method provided by the invention is applied to the recycling of nonwoven wool fiber or waste wool fiber to prepare active carbon. With a remarkably large specific surface area, the active carbon has the advantages of relatively high compatibility, good adsorption capacity, uniform void volume distribution and the like in the using process.
Description
Technical field
The present invention relates to a kind of high preparation method running through many microporous particles activated carbon, belong to recovery or the reprocessing technical field of waste material.
Background technology
Waste fiber stock number is huge, deals with improperly and not only results in environmental pollution, and can increase processing cost, wastes resource.Use proper method that waste textile fiber is reprocessed the requirement not only conforming with China's relevant laws regulation, and there is the reasonability of twice laid, resource reclaim.Discarded wool fibre includes spinning wool fibre (such as Pilus Sus domestica, Crinis Carbonisatus, chicken feather, Pilus Caprae seu Ovis or rabbit hair leftover bits and pieces, Pilus Cameli, alpaca fibre, cashmere pin hair etc.) and discarded wool fibre material (the woollen hard waste such as textile mills, lap waste, selvedge, waste wool yarn leftover pieces, old woollen clothes, old sweater etc.).The latest data announced in 82nd international wool manufacturing tissue annual meeting shows, 2013/2014 annual global only production of wool is contemplated to 1,100,000 tons of clean hairs, also can reflect that from this discarded wool fibre stock number is huge.Therefore, the most rationally disposing or recycle discarded wool fibre resource is the important topic currently faced.
In terms of the discarded wool fibre utilization of resources, mainly have two utilization orientation: one be use shredding, clean, screen, after directly utilize or through textile process, form the physics reuse method of available textile, remove the ethinylestradiol pollutant in sewage as Chinese patent CN102167418B discloses the adsorptive reactor utilized with waste wool fiber as filler；Two is cleaning, dissolving, form keratin liquid-purifying to utilize or regeneration spinning, textile process, form textile or pulverizing, the Chemical Physics method of absorption class material is made in carbonization, as Chinese patent CN 102161485 B utilizes waste wool to prepare tubular structure activated carbon, but this patent has the disadvantage that tubular structure easily bursts into fragments, the penetrability of outer wall activation micropore is poor, causes activated carbon specific surface area less, and absorbability is poor；In addition this patent cleans waste wool merely with water, it is impossible to the fat that shown by Pilus Caprae seu Ovis, the Chinese etc. are removed, and is unfavorable for activating the generation of micropore, thus affects the raising of the specific surface area of activated carbon.Cashmere pin hair results from goat depilation operation, diameter Distribution wider range, thickness skewness, thicker fiber is up to 170 μm, and the existing solid construction in fibre section, also has cavernous structure, it is a kind of Typical Representative in discarded wool fibre, the rare report of application to this obsolete material.
Based on this, make the application.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method utilizing cashmere pin wool fibre preparation height to run through many microporous particles activated carbon; alleviate environment to offal treatment pressure while; obtaining height and run through many microporous particles activated carbon, turn waste into wealth, meet resource maximally utilizes principle.
The present invention uses following technology path:
A kind of method utilizing cashmere pin wool fibre preparation height to run through many microporous activated carbon, comprises the steps:
Step one, cashmere pin wool fibre pretreatment stage, wool fibre will be discarded and be placed in the sulfuric acid solution of 2.5%-5.0% process, between 100 DEG C-115 DEG C, carbonization is bakeed after rolling acid, recycle broken charcoal machine removing vegetalitas grass miscellaneous, then neutralize, add nonionic detergent and remove the lanoline of discarded wool fibre, finally clean post-drying with 35-55 DEG C of hot water, it is thus achieved that clean cashmere pin wool fibre；
Step 2, the pre-carbonization stage of cashmere pin wool fibre; i.e. utilize lipper that clean cashmere pin wool fibre is cut into 5mm-15mm undercoat; it is placed under nitrogen protection in quartz tube type Muffle furnace; after logical nitrogen 30min; it is warming up between 200 DEG C-255 DEG C; pre-carbonization processes 30min to 90min, takes out, i.e. obtain the pre-carbonizing production of different structure form after being cooled to room temperature；
Step 3, pre-carbonizing production carbonization-activation stage; will mix with certain proportion according to mass ratio with activator by pre-carbonized product; it is placed in quartz tube type Muffle furnace under nitrogen protection; after logical nitrogen 30min; it is warming up between 500 DEG C-900 DEG C, then is incubated 60min to 150min, be cooled to room temperature and take out; cleaning to cleanout fluid pH value with 80 DEG C of hot water is between 5.8-7.5, and being i.e. able to cashmere pin wool fibre after filtering drying is the activated carbon of raw material.
Wherein, in described step one, cashmere pin wool fibre is the Typical Representative of discarded wool fibre; other can not be able to be spun wool fibre (such as Pilus Sus domestica, Crinis Carbonisatus, chicken feather, Pilus Caprae seu Ovis or rabbit hair leftover bits and pieces, Pilus Cameli, alpaca fibre etc.) and discarded wool fibre material (the woollen hard waste such as textile mills; lap waste; selvedge, waste wool yarn leftover pieces, old woollen clothes, old sweater etc.) replace cashmere pin wool fibre and carry out running through the preparation of many microporous particles activated carbon；The pretreating process flow process of cashmere pin wool fibre pretreatment stage is: containing the discarded wool fibre of grass → soak, roll acid → bakings → carbon removal → neutralize → go fat → drying → discard clean hair；Nonionic detergent refers to the one in Lissapol TN 450, Teric N10, Antarox C0630 and FK-9502 type nonionic detergent；The fat washing process technology controlling and process is gone to be: between concentration 0.5% to 2%, bath raio 1:15-55, temperature 45 C-60 DEG C, washing times 2 times, wash time is distributed as 10min, 5min；
In described step 2, heating rate is 5-15 DEG C/min；
In described step 3, pre-carbonized product should be less than 2 with the mixing quality ratio of activator；Heating rate is 5-15 DEG C/min；Activator refers to K2CO3、Na2CO3、Li2CO3、H3PO4
、KOH、NaOH、KOH- K2CO3、NaOH- Na2CO3In one.
The invention has the beneficial effects as follows:
The present invention utilizes pretreatment process to eliminate the fat on surface of discarded wool fibre, the Chinese, the most pre-carbonization, the formation of carbonization-activation process microcellular structure well；Furthermore by pre-carbonization, carbonization-activation process control, make discarded wool fibre granular active carbon have highly to run through, activation micropore is obvious, and stable network-like structure, drastically increase the specific surface area of activated carbon, enhance absorbability, to apply in heavy metal as high-efficiency adsorbent, organic dyestuff, harmful chemical processes, the fields such as the cleaning harmful gas such as water and formaldehyde, on the one hand this decrease and process the environmental pollution that discarded wool fibre brings, reduce again the processing cost of waste wool, waste resource is turned waste into wealth simultaneously, enrich waste resource and process the approach utilized.
The application is by pre-carbonization, pre-carbonization-activation process control; with cashmere pin wool fibre as raw material; height can be prepared and run through many microporous particles activated carbon; the method that cashmere pin hair preparation height also can run through many microporous particles activated carbon is applied in process and the application of other discarded wool fibres with technique; this is conducive to alleviating environment to offal treatment pressure; and the Appropriate application for discarded wool fibre provides more effective ways, thus improve product utilization added value.
Accompanying drawing explanation
Fig. 1 is the work flow schematic diagram of the present invention；
Fig. 2 is the view in the application before discarded cashmere pin hair pretreatment；
Fig. 3 is the discarded cashmere pretreated view of pin hair in the application；
Fig. 4 is to discard cashmere pin hair granular active carbon scanning electron microscope (SEM) photograph after middle carbonization-activation under the first enforcement state of the application；
Fig. 5 is the partial enlarged drawing of aminoacyl site in Fig. 4；
Fig. 6 is to discard cashmere pin hair granular active carbon scanning electron microscope (SEM) photograph after middle carbonization-activation under the application the second enforcement state；
Fig. 7 is the partial enlarged drawing at B position in Fig. 6；
Fig. 8 is to discard cashmere pin hair granular active carbon scanning electron microscope (SEM) photograph after middle carbonization-activation under the third enforcement state of the application；
Fig. 9 is the partial enlarged drawing at C position in Fig. 8.
Detailed description of the invention
In discarded wool fibre data as a example by cashmere pin hair, in conjunction with specific embodiments, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate the present invention rather than limit the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, the present invention can be made various changes or modifications by those skilled in the art, and these equivalent form of values fall within the application appended claims limited range equally.
Embodiment 1
The process technique of the present embodiment refers to shown in Fig. 1, discarded cashmere pin wool fibre is placed in sulfuric acid treatment in the sulfuric acid solution of 3.0%, carbonization is bakeed at 110 DEG C after rolling acid, recycle broken charcoal machine removing vegetalitas grass miscellaneous, then neutralize, add Teric N10 nonionic detergent (concentration 1.5%, bath raio 1:35, temperature 50 C, washing times twice, twice wash time is distributed as 10min, 5min) remove the lanoline of cashmere pin wool fibre, finally clean post-drying with 40 DEG C of hot water, obtain clean cashmere pin wool fibre, comparison diagram 2 and Fig. 3 can be seen that, fiber hair coloured light after purified treatment is bright neatly, and glossy degree height；Then utilizing lipper that clean cashmere pin wool fibre is cut into 15mm undercoat, be placed under nitrogen protection in quartz tube type Muffle furnace, after logical nitrogen 30min, be warming up to 255 DEG C with 15 DEG C/min, pre-carbonization processes 30min, is cooled to room temperature, and rear taking-up obtains pre-carbonizing production；Again by pre-carbonized product and Na2CO3Activator mixes with 1:1 certain proportion according to mass ratio; it is placed in quartz tube type Muffle furnace under nitrogen protection; after logical nitrogen 30min; it is warming up to 500 DEG C with 5 DEG C/min; it is incubated 100min again; being cooled to room temperature take out, cleaning to cleanout fluid pH value with 80 DEG C of hot water is about 6.8, and being i.e. able to cashmere pin wool fibre after filtering drying is the activated carbon of raw material.
Fig. 4 and Fig. 5 is to use the method described in the present embodiment to prepare cashmere pin hair granular active carbon electron-microscope scanning figure under different amplification; it is observed that the cashmere pin hair granular active carbon of the active micropore of part; but activation effect is abundant not, and activation micropore is less.It is 370.04m according to measuring its BET specific surface area2·g-1, average pore volume is 0.138cm3·g-1。
Embodiment 2
The process technique of the present embodiment refers to shown in Fig. 1, discarded cashmere pin wool fibre is placed in sulfuric acid treatment in the sulfuric acid solution of 3.5%, carbonization is bakeed at 105 DEG C after rolling acid, recycle broken charcoal machine removing vegetalitas grass miscellaneous, then neutralize, add Lissapol TN 450 nonionic detergent (concentration 1%, bath raio 1:50, temperature 55 DEG C, washing times twice, twice wash time is distributed as 10min, 5min) remove the lanoline of cashmere pin wool fibre, finally clean post-drying with 40 DEG C of hot water, obtain clean cashmere pin wool fibre, comparison diagram 2 and Fig. 3 can be seen that, fiber hair coloured light after purified treatment is bright neatly, and glossy degree height；Then utilizing lipper that clean cashmere pin wool fibre is cut into 10mm undercoat, be placed under nitrogen protection in quartz tube type Muffle furnace, after logical nitrogen 30min, be warming up to 250 DEG C with 5 DEG C/min, pre-carbonization processes 60min, is cooled to room temperature, and rear taking-up obtains pre-carbonizing production；Again by pre-carbonized product and K2CO3Activator mixes with 4:2 according to mass ratio; it is placed in quartz tube type Muffle furnace under nitrogen protection; after logical nitrogen 30min; it is warming up to 500 DEG C with 5 DEG C/min; it is incubated 150min again; being cooled to room temperature take out, cleaning to cleanout fluid pH value with 80 DEG C of hot water is about 6.2, and being i.e. able to cashmere pin wool fibre after filtering drying is the activated carbon of raw material.
Fig. 6 and Fig. 7 is to use the method described in the present embodiment to prepare cashmere pin hair granular active carbon electron-microscope scanning figure under different amplification; can be observed to define inside and there is a large amount of granular active carbon activating micropore; outside is done the exodermis such as the scale structure layer parcel of carbonization; this have impact on the adsorption effect of activated carbon to a certain extent, but outer wrap layer segment position starts activation microcellular structure occur.It is 526.54m according to measuring its BET specific surface area2·g-1, average pore volume is 0. 201cm3·g-1。
Embodiment 3
The process technique of the present embodiment refers to shown in Fig. 1, discarded cashmere pin wool fibre is placed in sulfuric acid treatment in the sulfuric acid solution of 3.5%, carbonization is bakeed at 105 DEG C after rolling acid, recycle broken charcoal machine removing vegetalitas grass miscellaneous, then neutralize, add Lissapol TN 450 nonionic detergent (concentration 1%, bath raio 1:50, temperature 55 DEG C, washing times twice, twice wash time is distributed as 10min, 5min) remove the lanoline of cashmere pin wool fibre, finally clean post-drying with 40 DEG C of hot water, obtain discarded clean wool fibre, comparison diagram 2 and Fig. 3 can be seen that, fiber hair coloured light after purified treatment is bright neatly, and glossy degree height；Then utilizing lipper that clean cashmere pin wool fibre is cut into 5mm undercoat, be placed under nitrogen protection in quartz tube type Muffle furnace, after logical nitrogen 30min, be warming up to 240 DEG C with 10 DEG C/min, pre-carbonization processes 60min, is cooled to room temperature, and rear taking-up obtains pre-carbonizing production；Again by pre-carbonized product and Na2CO3-NaOH composite activating agent mixes with 4:2 according to mass ratio; it is placed in quartz tube type Muffle furnace under nitrogen protection; after logical nitrogen 30min; it is warming up to 600 DEG C with 5 DEG C/min; it is incubated 120min again; being cooled to room temperature take out, cleaning to cleanout fluid pH value with 80 DEG C of hot water is about 6.0, and being i.e. able to cashmere pin wool fibre after filtering drying is the activated carbon of raw material.
Fig. 8 and Fig. 9 is to use the method described in the present embodiment to prepare cashmere pin hair granular active carbon electron-microscope scanning figure under different amplification; can be observed to define a large amount of granular active carbon activating micropore; oarse-grained activated carbon resolves into the granular active carbon of more small particle; and the exodermis such as wool scale layer obtains more activation microcellular structure after carbonization, this specific surface area contributing to increasing activated carbon.It is 736.9m according to measuring its BET specific surface area2·g-1, average pore volume is 0. 291cm3·g-1。
From above-mentioned preparation process it can be seen that prepare best results when embodiment 3.Activated carbon prepared under the program has the highest specific surface area, and during use, the compatibility is higher, and absorbability is good, and voidage is evenly distributed.
Above content is the further description that provided technical scheme is made by the preferred implementation combining the invention; it cannot be assumed that the invention is embodied as being confined to these explanations above-mentioned; for the invention person of an ordinary skill in the technical field; without departing from the concept of the premise of the invention; some simple deduction or replace can also be made, all should be considered as belonging to the protection domain of the invention.
Claims (10)
1. the one kind high preparation method running through many microporous particles activated carbon, it is characterised in that with discarded wool fibre as raw material, carries out the process of following steps:
(1) pretreatment is purified: after discarded wool fibre is placed in sulfuric acid solution process, rolls acid and bakee carbonization, remove impurity, then neutralize, add nonionic detergent and remove lanoline, finally clean with 35-55 DEG C of water, then dry, it is thus achieved that clean wool fibre；
(2) pre-carbonization: clean wool fibre is cut into broken section, is warming up to 200 DEG C-255 DEG C under nitrogen protection, and pre-carbonization processes 30-90min, is cooled to room temperature, obtains pre-carbonizing production；
(3) activation: be mixed in proportion with activator by pre-carbonized product, is warming up to 500 DEG C-900 DEG C under nitrogen protection, then is incubated 60-150min, be cooled to room temperature, and cleaning to cleanout fluid pH value is 5.8-7.5, and filtering drying, get product activated carbon.
A kind of high preparation method running through many microporous particles activated carbon the most as claimed in claim 1, it is characterised in that: in step (1), described sulfuric acid solution concentration is 2.5-5.0%；Bakee carbonization temperature and be 100-115 DEG C.
A kind of high preparation method running through many microporous particles activated carbon the most as claimed in claim 1, it is characterised in that in step (1), described nonionic detergent is Lissapol
TN 450, Teric N10 and Antarox C0630.
A kind of high preparation method running through many microporous particles activated carbon the most as claimed in claim 1, it is characterised in that described removal lanoline washing process technology controlling and process is as follows: the concentration of nonionic detergent is 0.5-2%, bath raio 1:10-30, temperature 45 C-55 DEG C.
5. a kind of high preparation method running through many microporous particles activated carbon as described in any one of claim 1-4, it is characterised in that: washing in described removal lanoline washing process and at least carry out 2 times, wash time is distributed as 10min, 5min.
A kind of high preparation method running through many microporous particles activated carbon the most as claimed in claim 1, it is characterised in that: in step (2), heating rate is 5-15 DEG C/min.
A kind of high preparation method running through many microporous particles activated carbon the most as claimed in claim 1, it is characterised in that: in step (3), described activator is KOH, NaOH, K2CO3, Na2CO3, Li2CO3、H3One in PO4, KOH-K2CO3, NaOH-Na2CO3.
A kind of high preparation method running through many microporous particles activated carbon the most as claimed in claim 1, it is characterised in that: in step (3), heating rate is 5-15 DEG C/min.
9. a kind of high preparation method running through many microporous particles activated carbon as described in claim 1,7 or 8, it is characterised in that: in step (3), described pre-carbonized product is less than 2 with the mixing quality ratio of activator.
A kind of high preparation method running through many microporous particles activated carbon the most as claimed in claim 1, it is characterised in that: described waste and old wool fibre is cashmere pin wool fibre, can not spin wool fibre or discarded wool fibre material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110170300A (en) * | 2019-05-08 | 2019-08-27 | 昆明理工大学 | A kind of preparation method of chicken feather modified honeycomb shape active carbon with high specific surface area adsorbent material |
| CN111554888A (en) * | 2020-04-09 | 2020-08-18 | 天津工业大学 | Anode material containing rabbit hair hollow carbon fibers for lithium-sulfur battery and preparation method thereof |
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| CN102660392A (en) * | 2012-05-29 | 2012-09-12 | 西北民族大学 | Detergent for wool |
| CN102838112A (en) * | 2012-09-26 | 2012-12-26 | 湘潭大学 | Preparation method of activated carbon |
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2016
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| CN102660392A (en) * | 2012-05-29 | 2012-09-12 | 西北民族大学 | Detergent for wool |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110170300A (en) * | 2019-05-08 | 2019-08-27 | 昆明理工大学 | A kind of preparation method of chicken feather modified honeycomb shape active carbon with high specific surface area adsorbent material |
| CN111554888A (en) * | 2020-04-09 | 2020-08-18 | 天津工业大学 | Anode material containing rabbit hair hollow carbon fibers for lithium-sulfur battery and preparation method thereof |
| CN111554888B (en) * | 2020-04-09 | 2022-04-29 | 天津工业大学 | Anode material containing rabbit hair hollow carbon fibers for lithium-sulfur battery and preparation method thereof |
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Application publication date: 20161012 |