CN104176736A - Method for preparing activated carbon from ionic liquid pretreated raw material - Google Patents
Method for preparing activated carbon from ionic liquid pretreated raw material Download PDFInfo
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- CN104176736A CN104176736A CN201410405528.7A CN201410405528A CN104176736A CN 104176736 A CN104176736 A CN 104176736A CN 201410405528 A CN201410405528 A CN 201410405528A CN 104176736 A CN104176736 A CN 104176736A
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- raw material
- gac
- ionic liquid
- activated carbon
- pyrrolidone
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Abstract
The invention relates to a method for preparing activated carbon from an ionic liquid pretreated raw material. The method is characterized by comprising the following steps: cleaning, drying and crushing forestry and agricultural residues which are used for preparing activated carbon, mixing with pyrrolidone acidic ionic liquid, stirring for 10-300 minutes at 30-100 DEG C, and then filtering to obtain a pretreated material; uniformly mixing the pretreated material with H3PO4, immersing in distilled water and stirring for 2 hours, drying in a constant-temperature air dry oven at 105 DEG C, putting into a tubular furnace after solidification, and activating a mixed material under the protection of N2; firstly dipping in 1mol/L hydrochloric acid solution for 2 hours after cooling, then washing by using hot distilled water until the pH value is unchanged, and drying in the constant-temperature air dry oven at 110 DEG C to obtain activated carbon. In the preparation process, activation is directly performed and a carbonization process is not needed, the defect that a conventional process adopts a great number of activating agents for preparing activated carbon can be overcome, the process is simple, the ionic liquid can be recycled, environment-friendly effect is achieved and pollution is less.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of method of preparing gac with ionic liquid pretreatment raw material.
Technical background
Gac is as porous adsorbing material, has abundant pore texture, higher specific surface area, good absorption property and stable chemical property, is widely used in the fields such as chemical industry, medical treatment, military affairs, environmental protection.
Most gac preparations need to be passed through carbonization process and reactivation process, and research contents mainly concentrates on the research of the aspects such as raw material, activating process, activator, less to the pre-treatment report of raw material.
Ionic liquid is generally by the asymmetric organic cation of the relatively large structure of specific volume and relatively little inorganic of volume or organic anion forms, be liquid state at room temperature or near room temperature temperature salt, conventionally also referred to as room-temperature ion.Liquid ions liquid is owing to having some unique performances, as has non-combustible, non-volatile, recoverable, and most compounds had to the advantages such as good solubility and be widely used in each research field.In pyrrolidinone compounds presence of acidic ionic liquid catalyst cellulose hydrolysis reaction process, can make cellulosic dehydration carbonization, as the people such as Feng Jianping (Feng Jianping, Liu Min, Guo Xinwen etc., pyrrolidone acidic ion liquid efficient catalytic cellulose hydrolysis glucose processed [J]. petroleum journal (refining of petroleum), 2012,28(5): 775-782.) think that pyrrolidinone compounds acidic ion liquid is the catalyzer of the promotion cellulose hydrolysis better than imidazoles acidic ion liquid.Through pyrrolidinone compounds acidic ion liquid pretreating raw material, can reduce without carbonization process direct activation, and can reduce the use of activator, reduce the corrosion of equipment and the harm to environment.
Have not yet to see the relevant report of preparing gac with ionic liquid pretreatment raw material.
Summary of the invention
The invention provides a kind of method of preparing gac with ionic liquid pretreatment raw material, with ionic liquid pretreatment raw material direct activation, prepare gac.
For achieving the above object, the present invention adopts following technical scheme:
(1) 100～200 orders are cleaned, are dried, are crushed to the agriculture and forestry organic waste material of preparing gac; The raw material crushing is mixed according to mass ratio 10:1～50 with pyrrolidinone compounds acidic ion liquid, and filter stir 10～300min at 30 ℃～100 ℃ temperature after, filtrate can be carried out next time and be used.
(2) by good raw material and the H of step (1) pre-treatment
3pO
4according to 1～6:1 mass ratio, evenly mix, adding distil water submergence is also stirred after 2h, dry in the constant temperature blast drying ovens of 105 ℃, puts into tube furnace, at N after solidifying
2protection under compound is activated, under 300～600 ℃ of activation temperatures, be incubated 30-100min.
(3) after cooling, gac is first soaked to 2h with 1mol/L hydrochloric acid soln, reusable heat distilled water wash is constant to pH, puts into 110 ℃ of constant temperature blast drying ovens and dries, and obtains gac.
Pyrrolidinone compounds acidic ion liquid described in step of the present invention (1) is 1-Methyl-2-Pyrrolidone hydrosulfate ([Hnmp] HSO
4), 1-Methyl-2-Pyrrolidone villaumite ([Hnmp] Cl), 1-Methyl-2-Pyrrolidone metilsulfate ([Hnmp] CH
3sO
3) in the mixing of one or more arbitrary proportions.
Agriculture and forestry organic waste material of the present invention refers to Seed of Chinese Soapberry shell, tealeaf residue, rice husk, palm hull, bamboo chip or wood chip.
The invention has the advantages that preparation process directly activates without carbonization process, overcome traditional technology and prepared the shortcoming that gac is used activator in a large number to there is the advantages such as technique is simple, ionic liquid can reuse, environmentally friendly, pollution is few.
Embodiment
Be below several specific embodiment of the present invention, further illustrate the present invention, but the present invention be not limited only to this.
Embodiment 1
100 orders are cleaned, are dried, are crushed to Seed of Chinese Soapberry residue; By the 1-Methyl-2-Pyrrolidone hydrosulfate of the raw material 100g crushing and 100g ([Hnmp] HSO
4) mix, and stir 60min at 50 ℃ of temperature, stir and finish rear filtration.By the good raw material 60g of pre-treatment and the H of 20g
3pO
4mix, adding distil water submergence is also stirred after 2h, dry in the constant temperature blast drying ovens of 105 ℃, puts into tube furnace, at N after solidifying
2under protection, compound is activated, under 400 ℃ of activation temperatures, be incubated 60min, temperature rise rate is 10 ℃/min.After cooling, gac is first soaked to 2h with 1mol/L hydrochloric acid soln, reusable heat distilled water wash is constant to pH, puts into 110 ℃ of constant temperature blast drying ovens and dries, and obtains gac sample.Prepared gac has following performance: BET specific surface area reaches 1498m
2/ g, methylene blue adsorption value 244mg/g.
Embodiment 2
200 orders are cleaned, are dried, are crushed to tealeaf residue; By the 1-Methyl-2-Pyrrolidone hydrosulfate of the raw material 100g crushing and 200g ([Hnmp] HSO
4), the 1-Methyl-2-Pyrrolidone villaumite ([Hnmp] Cl) of 50g mixes, and stirs 60min at 90 ℃ of temperature, stir and finish rear filtration.By the good raw material 60g of pre-treatment and the H of 10g
3pO
4mix, adding distil water submergence is also stirred after 2h, dry in the constant temperature blast drying ovens of 105 ℃, puts into tube furnace, at N after solidifying
2under protection, compound is activated, under 600 ℃ of activation temperatures, be incubated 60min.After cooling, gac is first soaked to 2h with 1mol/L hydrochloric acid soln, reusable heat distilled water wash is constant to pH, puts into 110 ℃ of constant temperature blast drying ovens and dries, and obtains gac sample.Prepared gac has following performance: BET specific surface area reaches 1156m
2/ g, methylene blue adsorption value 207mg/g.
Embodiment 3
100 orders are cleaned, are dried, are crushed to wood chip; By 1-Methyl-2-Pyrrolidone metilsulfate ([Hnmp] CH of the 1-Methyl-2-Pyrrolidone villaumite of the raw material 100g crushing and 300g ([Hnmp] Cl), 100g
3sO
3) mix, and stir 200min at 90 ℃ of temperature, stir and finish rear filtration.By the good raw material 60g of pre-treatment and the H of 50g
3pO
4mix, adding distil water submergence is also stirred after 2h, dry in the constant temperature blast drying ovens of 105 ℃, puts into tube furnace, at N after solidifying
2under protection, compound is activated, under 550 ℃ of activation temperatures, be incubated 100min.After cooling, gac is first soaked to 2h with 1mol/L hydrochloric acid soln, reusable heat distilled water wash is constant to pH, puts into 110 ℃ of constant temperature blast drying ovens and dries, and obtains gac sample.Prepared gac has following performance: BET specific surface area reaches 893m
2/ g, methylene blue adsorption value 175mg/g.
Embodiment 4
150 orders are cleaned, are dried, are crushed to bamboo chip; By the 1-Methyl-2-Pyrrolidone metilsulfate of the raw material 100g crushing and 300g ([Hnmp] CH
3sO
3) mix, and stir 300min at 60 ℃ of temperature, stir and finish rear filtration.By the good raw material 60g of pre-treatment and the H of 30g
3pO
4evenly mix, adding distil water submergence is also stirred after 2h, dry in the constant temperature blast drying ovens of 105 ℃, puts into tube furnace, at N after solidifying
2under protection, compound is activated, under 500 ℃ of activation temperatures, be incubated 60min.After cooling, gac is first soaked to 2h with 1mol/L hydrochloric acid soln, reusable heat distilled water wash is constant to pH, puts into 110 ℃ of constant temperature blast drying ovens and dries, and obtains gac sample.Prepared gac has following performance: BET specific surface area reaches 1779m
2/ g, methylene blue adsorption value 253mg/g.
Embodiment 5
Palm hull is cleaned, is dried to constant weight, is crushed to 120 orders; By the 1-Methyl-2-Pyrrolidone hydrosulfate of the raw material 100g crushing and 200g ([Hnmp] HSO
4), the 1-Methyl-2-Pyrrolidone villaumite ([Hnmp] Cl) of 100g, 1-Methyl-2-Pyrrolidone metilsulfate ([Hnmp] CH of 50g
3sO
3) mix, and add the submergence of 50ml distilled water, and stir 200min at 45 ℃ of temperature, stir and finish rear filtration.By the good raw material 60g of pre-treatment and the H of 60g
3pO
4mix, adding distil water submergence is also stirred after 2h, dry in the constant temperature blast drying ovens of 105 ℃, puts into tube furnace, at N after solidifying
2under protection, compound is activated, under 600 ℃ of activation temperatures, be incubated 90min.After cooling, gac is first soaked to 2h with 1mol/L hydrochloric acid soln, reusable heat distilled water wash is constant to pH, puts into 110 ℃ of constant temperature blast drying ovens and dries, and obtains gac sample.Prepared gac has following performance: BET specific surface area reaches 2051m
2/ g, methylene blue adsorption value 407mg/g.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing 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 (3)
1. with ionic liquid pretreatment raw material, prepare a method for gac, it is characterized in that:
(1) 100～200 orders are cleaned, are dried, are crushed to the agriculture and forestry organic waste material of preparing gac; The raw material crushing is mixed according to mass ratio 10:1～50 with pyrrolidinone compounds acidic ion liquid, and filter stir 10～300min at 30 ℃～100 ℃ temperature after;
(2) by good raw material and the H of step (1) pre-treatment
3pO
4according to 1～6:1 mass ratio, evenly mix, adding distil water submergence is also stirred after 2h, dry in the constant temperature blast drying ovens of 105 ℃, puts into tube furnace, at N after solidifying
2protection under compound is activated, under 300～600 ℃ of activation temperatures, be incubated 30-100min;
(3) after cooling, gac is first soaked to 2h with 1mol/L hydrochloric acid soln, reusable heat distilled water wash is constant to pH, puts into 110 ℃ of constant temperature blast drying ovens and dries, and obtains gac.
2. according to claim 1 a kind of
withionic liquid pretreatment raw material is prepared the method for gac, it is characterized in that described pyrrolidinone compounds acidic ion liquid is the mixing of one or more arbitrary proportions in 1-Methyl-2-Pyrrolidone hydrosulfate, 1-Methyl-2-Pyrrolidone villaumite, 1-Methyl-2-Pyrrolidone metilsulfate.
3. a kind of method of preparing gac with ionic liquid pretreatment raw material according to claim 1, is characterized in that described agriculture and forestry organic waste material refers to Seed of Chinese Soapberry shell, tealeaf residue, rice husk, palm hull, bamboo chip or wood chip.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106467296A (en) * | 2015-08-13 | 2017-03-01 | 明道学校财团法人明道大学 | Tea carbon and preparation method thereof |
| CN108128765A (en) * | 2017-12-26 | 2018-06-08 | 贵州大学 | Prepare method and the application of nitrogen-doped porous carbon material |
| CN109158083A (en) * | 2018-10-15 | 2019-01-08 | 西北师范大学 | A kind of preparation method and its usage of biomass-based carbon material |
| CN112973628A (en) * | 2021-02-06 | 2021-06-18 | 重庆文理学院 | Preparation method of activated carbon rich in basic functional groups |
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| CN101643207A (en) * | 2009-09-04 | 2010-02-10 | 江苏科技大学 | Method for preparing active carbon based on mulberry branch |
| CN102774837A (en) * | 2012-08-15 | 2012-11-14 | 福建农林大学 | Method for preparing activated carbon by taking ionic liquid as activator |
| CN103359729A (en) * | 2013-08-01 | 2013-10-23 | 中国科学院西双版纳热带植物园 | Novel preparation method of mesoporous active carbon |
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2014
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| CN101643207A (en) * | 2009-09-04 | 2010-02-10 | 江苏科技大学 | Method for preparing active carbon based on mulberry branch |
| CN102774837A (en) * | 2012-08-15 | 2012-11-14 | 福建农林大学 | Method for preparing activated carbon by taking ionic liquid as activator |
| CN103359729A (en) * | 2013-08-01 | 2013-10-23 | 中国科学院西双版纳热带植物园 | Novel preparation method of mesoporous active carbon |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106467296A (en) * | 2015-08-13 | 2017-03-01 | 明道学校财团法人明道大学 | Tea carbon and preparation method thereof |
| CN108128765A (en) * | 2017-12-26 | 2018-06-08 | 贵州大学 | Prepare method and the application of nitrogen-doped porous carbon material |
| CN108128765B (en) * | 2017-12-26 | 2021-04-30 | 贵州大学 | Method for preparing nitrogen-doped porous carbon material and application |
| CN109158083A (en) * | 2018-10-15 | 2019-01-08 | 西北师范大学 | A kind of preparation method and its usage of biomass-based carbon material |
| CN109158083B (en) * | 2018-10-15 | 2021-04-13 | 西北师范大学 | Preparation method and application of biomass-based carbon material |
| CN112973628A (en) * | 2021-02-06 | 2021-06-18 | 重庆文理学院 | Preparation method of activated carbon rich in basic functional groups |
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