CN107021482A - A kind of method that use carbon dioxide activation prepares terylene waste material matrix activated carbon - Google Patents
A kind of method that use carbon dioxide activation prepares terylene waste material matrix activated carbon Download PDFInfo
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- CN107021482A CN107021482A CN201710339057.8A CN201710339057A CN107021482A CN 107021482 A CN107021482 A CN 107021482A CN 201710339057 A CN201710339057 A CN 201710339057A CN 107021482 A CN107021482 A CN 107021482A
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- waste material
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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
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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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- 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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- 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
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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Abstract
The invention provides a kind of method that use carbon dioxide activation prepares terylene waste material matrix activated carbon, including one to terylene waste material the step of pre-process；Pretreated terylene waste material is transferred in tube furnace; nitrogen is passed through as protection gas; tube furnace is warming up to 300 ~ 500 DEG C of carbonation reaction temperature; reach and kept for 0.5 ~ 2 hour after carburizing temperature; the abundant high temperature pyrolysis of terylene waste material; after the completion of carbonization, in-furnace temperature is cooled to room temperature under nitrogen protection；Above-mentioned carbide is transferred under the conditions of tube furnace high temperature and carries out carbon dioxide activation, carbon dioxide flow is passed through for 100 ~ 500ml/min, carbon dioxide activation temperature is 600 ~ 900 DEG C, room temperature is cooled to after the completion of activation, activated carbon is washed with deionized to neutrality, activated carbon after washing is dried, so that activated carbon is made.884m is reached using activated carbon specific surface area made from the method for the present invention2/g。
Description
Technical field
The invention belongs to chemical field, it is related to the technology of preparing of a kind of textile waste recycling and activated carbon, specifically
For be a kind of method that use carbon dioxide activation prepares terylene waste material matrix activated carbon.
Background technology
Constantly increase with the demand of domestic polyester staple fiber, terylene waste material amount is also continuously increased, China's washing every year
Synthetic fibre weaving discarded object reaches millions of tons.They are buried or are incinerated, and have not only wasted resource but also have destroyed environment.One side
Face, they are difficult to be degraded by microorganisms；On the other hand during Polyester Textiles are prepared, used finishing agent or auxiliary is whole
The chemical compositions such as reason agent can be remained in Polyester Textiles, so as to endanger environment；3rd, annex or subsidiary on Polyester Textiles
Thing complicated component, it is very harmful.Therefore suitable method is needed to handle terylene textile waste, if can using terylene waste material come
Porous carbon is generated, the effect that changing waste into resources is utilized can be reached, the production cost of porous carbon can be reduced again.
Activated carbon has abundant pore structure and oxygen-containing functional group, it as adsorbent, catalyst carrier etc. and it is wide
General utilization.The activation of activation method Main physical, chemical activation and the physical-chemical activation of activated carbon.Utilize these tradition sides
Activated carbon hole prepared by method is difficult to control to, mesoporous less based on micropore and macropore, and part chemical activating agent is such as used
Zinc chloride activation method, which prepares activated carbon, can cause new pollution.
With the coal the reach of science in modern age, scientist develops the method for various control carbon material pore structures, chemistry
It is higher that method prepares activated carbon cost, and can cause environmental pollution.Therefore Physical prepares activated carbon and got growing concern for
And development.Activated carbon is prepared using Physical, the activated carbon containing a large amount of uniform mesopores can be not only obtained, and cost is relatively low,
Environmental pollution is smaller.
Patent 200910080981.4 discloses a kind of preparation method of activated carbon.Step is as follows:1) after will be broken, dry
Tobacco rod carbonized, obtain carbonizing production；2) it is carbonizing production progress is physically activated, obtain activated carbon.Utilize this hair
The charcoal absorption performance that bright method is prepared is good, and harmful substance contents are extremely low, and indices meet national standard,
Available for sewage disposal or chemical products, food, medicine decolouring.
Paper physical activation method prepares coconut shell based activated carbon and its pore structure develops Fan Zhuan army Tianjin:University Of Tianjin,
2008；21(3):Proposed in 11-14. using coconut husk as raw material, activated carbon is prepared using charing and vapor activation.It is made
Specific surface area is 502~819m2/ g's, pore size is 4~7nm activated carbon.
Find out from above-mentioned document, Physical preparation active carbon method is feasible, and the material property prepared is preferable.And physics
It is lower than chemical method that method prepares activated carbon cost, and environmental pollution is small.
The content of the invention
For above-mentioned technical problem of the prior art, terylene is prepared using carbon dioxide activation the invention provides one kind
The method of waste material matrix activated carbon, the method that described this use carbon dioxide activation prepares terylene waste material matrix activated carbon will be solved
Activated carbon hole prepared by art methods is difficult to control to, and ibid easily causes the technical problem of new pollution.
The invention provides a kind of method that use carbon dioxide activation prepares terylene waste material matrix activated carbon, including following step
Suddenly：
1) one the step of pre-processed to terylene waste material, after terylene waste material clean dry, crushing fragmentate it is standby,
The area of plane of described fragment is less than 1cm × 1cm；
2) one the step of be carbonized to terylene waste material, by step 1) in terylene waste material be transferred in tube furnace, lead to
Enter nitrogen as protection gas, stripping 15min-30min drains tubular type furnace air, tube furnace is warming up into carbonation reaction temperature
300~500 DEG C, heating rate is 5 DEG C/min-15 DEG C/min, reaches and is kept for 0.5~2 hour after carburizing temperature, terylene waste material fills
Divide high temperature pyrolysis, after the completion of carbonization, in-furnace temperature is cooled to room temperature under nitrogen protection；
3) one the step of activated to carbide, by step 2) in carbide be transferred to tube furnace high temperature condition
Lower carry out carbon dioxide activation, is passed through carbon dioxide flow for 100~500ml/min, and carbon dioxide activation temperature is 600~
900 DEG C, room temperature is cooled to after the completion of activation, activated carbon is washed with deionized to neutrality, the activated carbon after washing is placed in drum
Dried in wind drying box, so that activated carbon is made.
Further, in step 1) in, original terylene waste material is washed, dried, is then comminuted into.
Further, in terylene waste material carbonisation, will need to be passed through nitrogen as protection gas, nitrogen flow be 100~
300ml/min。
Further, the specific surface area of prepared activated carbon is 884m2/g。
The present invention weaves discarded object as carbon matrix precursor using terylene, and porous activated carbon is prepared by activator of carbon dioxide.
Terylene weaving discarded object high temperature pyrolysis, removes non-carbons material at 300 DEG C -500 DEG C, forms carbide.At 600 DEG C -900 DEG C
Under, the carbide for discarded object of being weaved using concentration for 99.5%-99.9% carbon dioxide activation terylene forms loose structure.
Activated carbon specific surface area reaches 884m made from this method2/g。
The relatively low terylene waste material of use value of the present invention is prepared into the activity with high added value by being pyrolyzed the method for activation
Charcoal, and applied in terms of adsorbing heavy metal in water.Compared with traditional chemical method prepares activated carbon, prepared and lived using carbon dioxide
Property charcoal, not only the pollution of cost low environment is small, and can prepare high-specific surface area and have the activated carbon of micro--meso-hole structure.Due to
Carbon dioxide activation is acted on so that activated carbon has higher specific surface area and abundant oxygen-containing functional group, to Cr6+Absorption effect
Fruit is very well.
The present invention is compared with prior art, and its technological progress is significant.Activated carbon is prepared the invention belongs to Physical, into
This is lower than chemical method, and environmental pollution is small.Discarded terylene is prepared into activated carbon by the present invention using carbon dioxide activation, further
Using activated carbon as sorbing material, it is found that heavy metal has excellent adsorption effect.The present invention both realizes changing waste into resources
Utilize the purpose for having reached the treatment of wastes with processes of wastes against one another again.
Brief description of the drawings
Fig. 1 is the graph of pore diameter distribution, specific surface area and pore volume of activated carbon in embodiments of the invention 5.
Fig. 2 is the ESEM (SEM) of activated carbon in embodiments of the invention 5.
Fig. 3 is transmission electron microscope (TEM) figure of activated carbon in embodiments of the invention 5.
Embodiment
In order that technological means, character of innovation, reached purpose and effect for realizing of the present invention are it can be readily appreciated that once embodiment
The method that prepared by a kind of carbon dioxide activation method to the present invention into terylene waste material matrix activated carbon is specifically addressed.
Embodiment 1
The pretreatment of terylene waste material:The small pieces that 1cm*1cm is cut into after terylene waste material clean dry are standby.Its ash content is
0.52, volatilization is divided into 88.39, and fixed carbon is 10.71, C, H, N, S percentage composition is respectively 63.51%, 5.11%,
6.43%th, 0.11%.
The carbonization of terylene waste material:Pretreated terylene waste material is transferred in tube furnace, under nitrogen protection with 10 DEG C/
Min speed, which is warming up to 300 DEG C and stopped after the completion of 1h, carbonization, is cooled to room temperature.
The activation of terylene waste material：Carbide is transferred in tube furnace, under nitrogen protection with 10 DEG C/min speed liter
Temperature starts to be passed through carbon dioxide, and stop 1h to 800 DEG C.Room temperature is cooled to after activation under nitrogen protection.Use deionization
Water washing activated carbon is 6~7 to pH, and the activated carbon after washing is placed in 105 DEG C of air dry oven and dries 12h, this is made
The activated carbon of embodiment.
Embodiment 2
The pretreatment of terylene waste material:The small pieces that 1cm*1cm is cut into after terylene waste material clean dry are standby.Its ash content is
0.52, volatilization is divided into 88.39, and fixed carbon is 10.71, C, H, N, S percentage composition is respectively 63.51%, 5.11%,
6.43%th, 0.11%.
The carbonization of terylene waste material:Pretreated terylene waste material is transferred in tube furnace, under nitrogen protection with 10 DEG C/
Min speed, which is warming up to 350 DEG C and stopped after the completion of 1h, carbonization, is cooled to room temperature.
The activation of terylene waste material：Carbide is transferred in tube furnace, under nitrogen protection with 10 DEG C/min speed liter
Temperature starts to be passed through carbon dioxide, and stop 1h to 800 DEG C.Room temperature is cooled to after activation under nitrogen protection.Use deionization
Water washing activated carbon is 6~7 to pH, and the activated carbon after washing is placed in 105 DEG C of air dry oven and dries 12h, this is made
The activated carbon of embodiment.
Embodiment 3
The pretreatment of terylene waste material:The small pieces that 1cm*1cm is cut into after terylene waste material clean dry are standby.Its ash content is
0.52, volatilization is divided into 88.39, and fixed carbon is 10.71, C, H, N, S percentage composition is respectively 63.51%, 5.11%,
6.43%th, 0.11%.
The carbonization of terylene waste material:Pretreated terylene waste material is transferred in tube furnace, under nitrogen protection with 10 DEG C/
Min speed, which is warming up to 400 DEG C and stopped after the completion of 1h, carbonization, is cooled to room temperature.
The activation of terylene waste material：Carbide is transferred in tube furnace, under nitrogen protection with 10 DEG C/min speed liter
Temperature starts to be passed through carbon dioxide, and stop 1h to 800 DEG C.Room temperature is cooled to after activation under nitrogen protection.Use deionization
Water washing activated carbon is 6~7 to pH, and the activated carbon after washing is placed in 105 DEG C of air dry oven and dries 12h, this is made
The activated carbon of embodiment.
Embodiment 4
The pretreatment of terylene waste material:The small pieces that 1cm*1cm is cut into after terylene waste material clean dry are standby.Its ash content is
0.52, volatilization is divided into 88.39, and fixed carbon is 10.71, C, H, N, S percentage composition is respectively 63.51%, 5.11%,
6.43%th, 0.11%.
The carbonization of terylene waste material:Pretreated terylene waste material is transferred in tube furnace, under nitrogen protection with 10 DEG C/
Min speed, which is warming up to 350 DEG C and stopped after the completion of 1h, carbonization, is cooled to room temperature.
The activation of terylene waste material：Carbide is transferred in tube furnace, under nitrogen protection with 10 DEG C/min speed liter
Temperature starts to be passed through carbon dioxide, and stop 1h to 750 DEG C.Room temperature is cooled to after activation under nitrogen protection.Use deionization
Water washing activated carbon is 6~7 to pH, and the activated carbon after washing is placed in 105 DEG C of air dry oven and dries 12h, this is made
The activated carbon of embodiment.
Embodiment 5
The pretreatment of terylene waste material:The small pieces that 1cm*1cm is cut into after terylene waste material clean dry are standby.Its ash content is
0.52, volatilization is divided into 88.39, and fixed carbon is 10.71, C, H, N, S percentage composition is respectively 63.51%, 5.11%,
6.43%th, 0.11%.
The carbonization of terylene waste material:Pretreated terylene waste material is transferred in tube furnace, under nitrogen protection with 10 DEG C/
Min speed, which is warming up to 350 DEG C and stopped after the completion of 1h, carbonization, is cooled to room temperature.
The activation of terylene waste material：Carbide is transferred in tube furnace, under nitrogen protection with 10 DEG C/min speed liter
Temperature starts to be passed through carbon dioxide, and stop 1h to 800 DEG C.Room temperature is cooled to after activation under nitrogen protection.Use deionization
Water washing activated carbon is 6~7 to pH, and the activated carbon after washing is placed in 105 DEG C of air dry oven and dries 12h, this is made
The activated carbon of embodiment.
Embodiment 6
The pretreatment of terylene waste material:The small pieces that 1cm*1cm is cut into after terylene waste material clean dry are standby.Its ash content is
0.52, volatilization is divided into 88.39, and fixed carbon is 10.71, C, H, N, S percentage composition is respectively 63.51%, 5.11%,
6.43%th, 0.11%.
The carbonization of terylene waste material:Pretreated terylene waste material is transferred in tube furnace, under nitrogen protection with 10 DEG C/
Min speed, which is warming up to 350 DEG C and stopped after the completion of 1h, carbonization, is cooled to room temperature.
The activation of terylene waste material：Carbide is transferred in tube furnace, under nitrogen protection with 10 DEG C/min speed liter
Temperature starts to be passed through carbon dioxide, and stop 1h to 850 DEG C.Room temperature is cooled to after activation under nitrogen protection.Use deionization
Water washing activated carbon is 6~7 to pH, and the activated carbon after washing is placed in 105 DEG C of air dry oven and dries 12h, this is made
The activated carbon of embodiment.
Simple illustration once is done to the data in drawing and form
Fig. 1 is the graph of pore diameter distribution, specific surface area and pore volume of activated carbon in embodiments of the invention 5.Fig. 2 is the present invention
Embodiment 5 in activated carbon ESEM (SEM).Fig. 3 is the transmission electron microscope (TEM) of activated carbon in embodiments of the invention 5
Figure.As shown in Figure 1, the terylene waste material matrix activated carbon specific surface area is higher, illustrates there is preferable absorption property, and main with micro-
Based on hole, be conducive to the absorption to small molecule contaminants.From Fig. 2 and Fig. 3, the terylene waste material matrix activated carbon surface has brighter
Aobvious pore structure, abundant pore structure is to assess one of good necessary condition of charcoal absorption performance.
Claims (4)
1. a kind of method that use carbon dioxide activation prepares terylene waste material matrix activated carbon, it is characterised in that comprise the following steps：
1）One the step of pre-processed to terylene waste material, after terylene waste material clean dry, crushing fragmentates standby, institute
The fragment stated is less than 1cm × 1cm；
2）One the step of be carbonized to terylene waste material, by step 1) in terylene waste material be transferred in tube furnace, be passed through nitrogen
Gas is as protection gas, and stripping 15min-30min drains tubular type furnace air, by tube furnace be warming up to carbonation reaction temperature 300 ~
500 DEG C, heating rate is 5 DEG C/min-15 DEG C/min, reaches and is kept for 0.5 ~ 2 hour after carburizing temperature, the abundant high temperature of terylene waste material
Pyrolysis, after the completion of carbonization, in-furnace temperature is cooled to room temperature under nitrogen protection；
3）One the step of activated to carbide, by step 2) in carbide be transferred to tube furnace high temperature under the conditions of enter
Row carbon dioxide activation, is passed through carbon dioxide flow for 100 ~ 500ml/min, and carbon dioxide activation temperature is 600 ~ 900 DEG C, living
Room temperature is cooled to after the completion of change, activated carbon is washed with deionized to neutrality, the activated carbon after washing is placed in air dry oven
Interior drying, so that activated carbon is made.
2. the method that a kind of use carbon dioxide activation as claimed in claim 1 prepares terylene waste material matrix activated carbon, its feature
It is：In step 1）In, original terylene waste material is washed, dried, is then comminuted into.
3. the method that a kind of use carbon dioxide activation as claimed in claim 1 prepares terylene waste material matrix activated carbon, its feature
It is：In terylene waste material carbonisation, nitrogen will need to be passed through as protection gas, and nitrogen flow is 100 ~ 300ml/min.
4. the method that a kind of use carbon dioxide activation as claimed in claim 1 prepares terylene waste material matrix activated carbon, its feature
It is：The specific surface area of prepared activated carbon is 884m2/g。
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| CN201710339057.8A CN107021482A (en) | 2017-05-15 | 2017-05-15 | A kind of method that use carbon dioxide activation prepares terylene waste material matrix activated carbon |
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| CN201710339057.8A CN107021482A (en) | 2017-05-15 | 2017-05-15 | A kind of method that use carbon dioxide activation prepares terylene waste material matrix activated carbon |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110127691A (en) * | 2018-02-02 | 2019-08-16 | 现代自动车株式会社 | Method for manufacturing active carbon |
| CN111082053A (en) * | 2019-12-30 | 2020-04-28 | 江南大学 | Carbon-based material and application thereof in lithium ion battery |
| CN114293364A (en) * | 2022-01-28 | 2022-04-08 | 华北电力大学（保定） | Carbon fiber activation method and apparatus |
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| CN1114287A (en) * | 1994-06-04 | 1996-01-03 | 王吉祥 | Method for continuously producing active carbon fibre cloth and device thereof |
| CN101508435A (en) * | 2009-03-31 | 2009-08-19 | 煤炭科学研究总院 | Process for producing active carbon |
| CN105384170A (en) * | 2015-10-28 | 2016-03-09 | 武汉纺织大学 | Method for preparing activated charcoal by utilizing waste textile fiber material in molten-salt medium |
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2017
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| CN1114287A (en) * | 1994-06-04 | 1996-01-03 | 王吉祥 | Method for continuously producing active carbon fibre cloth and device thereof |
| CN101508435A (en) * | 2009-03-31 | 2009-08-19 | 煤炭科学研究总院 | Process for producing active carbon |
| CN105384170A (en) * | 2015-10-28 | 2016-03-09 | 武汉纺织大学 | Method for preparing activated charcoal by utilizing waste textile fiber material in molten-salt medium |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110127691A (en) * | 2018-02-02 | 2019-08-16 | 现代自动车株式会社 | Method for manufacturing active carbon |
| CN111082053A (en) * | 2019-12-30 | 2020-04-28 | 江南大学 | Carbon-based material and application thereof in lithium ion battery |
| CN111082053B (en) * | 2019-12-30 | 2021-11-02 | 江南大学 | Carbon-based material and application thereof in lithium ion battery |
| CN114293364A (en) * | 2022-01-28 | 2022-04-08 | 华北电力大学（保定） | Carbon fiber activation method and apparatus |
| CN114293364B (en) * | 2022-01-28 | 2023-09-26 | 华北电力大学（保定） | Carbon fiber activation method and equipment |
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