CN106268718B - A kind of method and its application of modified activated carbon - Google Patents
A kind of method and its application of modified activated carbon Download PDFInfo
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- CN106268718B CN106268718B CN201610694252.8A CN201610694252A CN106268718B CN 106268718 B CN106268718 B CN 106268718B CN 201610694252 A CN201610694252 A CN 201610694252A CN 106268718 B CN106268718 B CN 106268718B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
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Abstract
The present invention relates to a kind of method and its application of modified activated carbon, belong to technical field of new material preparation.Active carbon addition concentrated nitric acid mixing return stirring is obtained into modified product I first；Thionyl chloride and DMF are uniformly mixed and obtain mixing organic liquor I, then mixing I electromagnetic agitation of organic liquor is added in modified product I, and drying obtains modified product II；Ethylenediamine and DMF are uniformly mixed and obtain mixing organic liquor II, mixing organic liquor II then is added in modified product II, electromagnetic agitation obtains modified product III；Tetrahydrofuran, triethylamine, chloracetyl chloride are uniformly mixed and obtain mixing organic liquor III, then modified product III is added mixing organic liquor III and stirs to get modified product IV；The addition of modified product IV stannous chloride, 4,4'- bipyridyl are obtained into mixture, vinyl imidazole and DMF are uniformly mixed and obtain mixing organic liquor IV, mixing organic liquor IV is added mixture into and modified activated carbon is prepared.The modified active carbon has bigger adsorbance relative to untreated active carbon.
Description
Technical field
The present invention relates to a kind of method and its application of modified activated carbon, belong to technical field of new material preparation.
Background technique
Waste water in dye production belongs to one of intractable industrial wastewater, this year, and the development of textile industry has driven dyestuff raw
The development of production.Investigation shows that the annual dyestuff in the whole world is more than 700,000 tons, wherein 2% is directly entered water body and is arranged in the form of waste water
Out, it 10% is lost during subsequent dope dyeing.Waste water from dyestuff complicated component, change of water quality is big, and coloration is deep, and concentration is big, place
Reason is difficult.
Active carbon is the black voluminous powder by carbonaceous material after being activated.It has internal voids prosperity, ratio
The features such as surface area is big, adsorption capacity is strong.Because its property is stablized, there are good heat resistance, and not soluble in water or organic solvent,
It is easy to regenerate, is a kind of environmentally friendly adsorbent.
It is structurally-modified modified with surface chemical property that activated carbon modified method is broadly divided into surface physics.The table of active carbon
Physical structure modification in face, which refers to, to be increased active carbon specific surface area by the method for physics in the preparation process of active carbon, changed
Micro pore volume and structure, adjustment pore-size distribution etc., to change the physical adsorption property of active carbon.Surface physics architectural characteristic changes
It is combined modified that property can be divided into physical modification, chemical modification and physical chemistry.In the modified method of surface chemical property, active carbon
Raw material determine the value volume and range of product of its surface functional group.Surface-active functional group's type and quantity of active carbon are to absorption
There is significant impact with catalysis.Modified acidity, the alkalinity for mainly changing activated carbon surface of surface chemical property, introduces or removes
Certain surface functional groups, to make active carbon that there is certain special absorption or catalytic performance.Currently used surface chemistries
The modified method of matter has modified Surface Oxidation Modification, surface reduction, load substance modification, high-temperature heat treatment and low temperature plasma
Processing etc..
The present invention mainly starts with from the chemical property for changing activated carbon surface, obtains active carbon to the end by grafting functional group
The positively charged Cationic functional groups in surface reach the dyestuff for eliminating negatively charged anionic functional group.
Summary of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides a kind of method of modified activated carbon and its answers
With.The active carbon is handled through chemical reagent such as pernitric acid, thionyl chloride, ethylenediamine, chloracetyl chloride, vinyl imidazoles and is modified, and is changed
Active carbon after property has bigger adsorbance relative to untreated active carbon；Since modified acticarbon is because of it
The different shown abilities for having Preferential adsorption to anionic dye come out of component, structure, the present invention is by the following technical programs
It realizes.
A kind of method of modified activated carbon, the specific steps of which are as follows:
(1) first by active carbon according to liquid-solid ratio be 100 ~ 150:20 ~ 25ml/g be added concentrated nitric acid mixing return stirring 10 ~
12h is washed to pH equal to 7 after reaction, and drying obtains modified product I；
(2) being that 10~15:40~60 are uniformly mixed according to volume ratio by thionyl chloride and DMF obtains mixing organic liquor I, so
The modified product I that step (1) is obtained afterwards is that mixing organic liquor I is added 60~80 in 50 ~ 75:19 ~ 25ml/g according to liquid-solid ratio
10~12h of electromagnetic agitation under conditions of DEG C, filters washed with DMF after reaction, and drying obtains modified product II；
(3) being that 10~20:40~50 are uniformly mixed according to volume ratio by ethylenediamine and DMF obtains mixing organic liquor II, so
It is afterwards that mixing organic liquor II is added in 47 ~ 54:19 ~ 24ml/g according to liquid-solid ratio by modified product II, under conditions of 60~80 DEG C
10~12h of electromagnetic agitation, washing drying obtain modified product III；
(4) it is that 40~60:4~8:3~6 are uniformly mixed according to volume ratio by tetrahydrofuran, triethylamine, chloracetyl chloride to obtain
Organic liquor III is mixed, the modified product III for then obtaining step (3) is that mixing is added in 45 ~ 50:18 ~ 24ml/g according to liquid-solid ratio
Organic liquor III stirs 10~12h under conditions of 40~50 DEG C, then is dried to obtain modified product IV with tetrahydrofuran wash clean；
(5) modified product IV for obtaining step (4) is that stannous chloride, 4 is added in 50 ~ 60:1 ~ 2:2 ~ 4 according to mass ratio,
4'- bipyridyl obtains mixture, and vinyl imidazole and DMF are mixed according to volume ratio for 5~10:50~70
Mixing organic liquor IV is added for 50 ~ 55:18 ~ 23ml/g according to liquid-solid ratio, in N in mixture by organic liquor IV224 are stirred in atmosphere
Modified activated carbon is prepared after filtration drying in~30h.
Concentrated nitric acid concentration is 60%~90% in the step (1).
The modified activated carbon application is in adsorpting anion dyestuff process as adsorbent.
The beneficial effects of the present invention are: the Costco Wholesale in view of active carbon is cheap, and to the adsorption rate of waste water from dyestuff
Height has very high use value suitable for the production of various enterprises in real life.
Detailed description of the invention
Fig. 1 is composite diagram of the present invention.
Specific embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
As shown in Figure 1, the method for the modified activated carbon, the specific steps of which are as follows:
(1) first by 100g active carbon according to liquid-solid ratio be 100:20ml/g be added concentrated nitric acid (concentrated nitric acid concentration is 60%g/
Ml return stirring 10h) is mixed, is washed to pH after reaction equal to 7, drying obtains modified product I；
(2) being that 10:40 is uniformly mixed according to volume ratio by thionyl chloride and DMF obtains mixing organic liquor I, then by step
(1) modified product I obtained is that mixing electromagnetic agitation under conditions of 60 DEG C of organic liquor I is added in 50:19ml/g according to liquid-solid ratio
10h is filtered washed with DMF after reaction, and drying obtains modified product II；
(3) being that 10:40 is uniformly mixed according to volume ratio by ethylenediamine and DMF obtains mixing organic liquor II, then will be modified
Product II is that mixing organic liquor II, electromagnetic agitation 10h under conditions of 60 DEG C is added in 47:19ml/g according to liquid-solid ratio, and washing is dried
It is dry to obtain modified product III；
(4) being that 40:4:3 is uniformly mixed according to volume ratio by tetrahydrofuran, triethylamine, chloracetyl chloride obtains mixing organic liquor
III, the modified product III for then obtaining step (3) is that mixing organic liquor III is added in 45:18ml/g according to liquid-solid ratio, at 40 DEG C
Under conditions of stir 10h, then dried to obtain modified product IV with tetrahydrofuran wash clean；
(5) modified product IV for obtaining step (4) is that stannous chloride is added in 50:1:2,4,4'- joins pyrrole according to mass ratio
Pyridine obtains mixture, and being that 5:50 is uniformly mixed according to volume ratio by vinyl imidazole and DMF obtains mixing organic liquor IV, will mix
Material is that mixing organic liquor IV is added in 50:18ml/g according to liquid-solid ratio, in N2It stirs in atmosphere for 24 hours, is prepared after filtration drying
Modified activated carbon.
Adsorb comparative test:
Configuration concentration is 100mg/L lemon yellow solution, and adjusting pH value is 1, weighs the not processed activity of 20mg respectively
The active carbon that charcoal and process the present embodiment are modified is added separately in 500ml, 100mg/L lemon yellow solution, not processed work
Property charcoal adsorption rate be 47.8%, be 75.3% by the modified activated carbon adsorption rate of the present embodiment.
Embodiment 2
As shown in Figure 1, the method for the modified activated carbon, the specific steps of which are as follows:
(1) first by 100g active carbon according to liquid-solid ratio be 150:25ml/g be added concentrated nitric acid (concentrated nitric acid concentration is 90%g/
Ml return stirring 12h) is mixed, is washed to pH after reaction equal to 7, drying obtains modified product I；
(2) being that 12:50 is uniformly mixed according to volume ratio by thionyl chloride and DMF obtains mixing organic liquor I, then by step
(1) modified product I obtained is that mixing electromagnetic agitation under conditions of 80 DEG C of organic liquor I is added in 75:25ml/g according to liquid-solid ratio
12h is filtered washed with DMF after reaction, and drying obtains modified product II；
(3) being that 15:45 is uniformly mixed according to volume ratio by ethylenediamine and DMF obtains mixing organic liquor II, then will be modified
Product II is that mixing organic liquor II, electromagnetic agitation 12h under conditions of 50 DEG C is added in 54:24ml/g according to liquid-solid ratio, and washing is dried
It is dry to obtain modified product III；
(4) being that 60:8:6 is uniformly mixed according to volume ratio by tetrahydrofuran, triethylamine, chloracetyl chloride obtains mixing organic liquor
III, the modified product III for then obtaining step (3) is that mixing organic liquor III is added in 50:24ml/g according to liquid-solid ratio, at 50 DEG C
Under conditions of stir 12h, then dried to obtain modified product IV with tetrahydrofuran wash clean；
(5) modified product IV for obtaining step (4) is that stannous chloride is added in 60:2:4,4,4'- joins pyrrole according to mass ratio
Pyridine obtains mixture, and being that 10:70 is uniformly mixed according to volume ratio by vinyl imidazole and DMF obtains mixing organic liquor IV, will mix
It is that mixing organic liquor IV is added in 55:23ml/g that material, which is closed, according to liquid-solid ratio, in N228h is stirred in atmosphere, is prepared into after filtration drying
To modified activated carbon.
Adsorb comparative test:
Configuration concentration is 100mg/L lemon yellow solution, and adjusting pH value is 1, weighs the not processed activity of 20mg respectively
The active carbon that charcoal and process the present embodiment are modified is added separately in 500ml, 100mg/L lemon yellow solution, not processed work
Property charcoal adsorption rate be 48.5% by the modified activated carbon adsorption rate of the present embodiment be 76.1%.
Embodiment 3
As shown in Figure 1, the method for the modified activated carbon, the specific steps of which are as follows:
(1) first by 100g active carbon according to liquid-solid ratio be 125:23ml/g be added concentrated nitric acid (concentrated nitric acid concentration is 80%g/
Ml return stirring 11h) is mixed, is washed to pH after reaction equal to 7, drying obtains modified product I；
(2) being that 15:60 is uniformly mixed according to volume ratio by thionyl chloride and DMF obtains mixing organic liquor I, then by step
(1) modified product I obtained is that mixing electromagnetic agitation under conditions of 70 DEG C of organic liquor I is added in 63:22ml/g according to liquid-solid ratio
11h is filtered washed with DMF after reaction, and drying obtains modified product II；
(3) being that 20:50 is uniformly mixed according to volume ratio by ethylenediamine and DMF obtains mixing organic liquor II, then will be modified
Product II is that mixing organic liquor II, electromagnetic agitation 11h under conditions of 70 DEG C is added in 51:22ml/g according to liquid-solid ratio, and washing is dried
It is dry to obtain modified product III；
(4) being that 50:6:5 is uniformly mixed according to volume ratio by tetrahydrofuran, triethylamine, chloracetyl chloride obtains mixing organic liquor
III, the modified product III for then obtaining step (3) is that mixing organic liquor III is added in 47:21ml/g according to liquid-solid ratio, at 45 DEG C
Under conditions of stir 11h, then dried to obtain modified product IV with tetrahydrofuran wash clean；
(5) modified product IV for obtaining step (4) is that stannous chloride is added in 55:1.5:3,4,4'- joins according to mass ratio
Pyridine obtains mixture, and being that 8:60 is uniformly mixed according to volume ratio by vinyl imidazole and DMF obtains mixing organic liquor IV, will mix
It is that mixing organic liquor IV is added in 53:21ml/g that material, which is closed, according to liquid-solid ratio, in N230h is stirred in atmosphere, is prepared into after filtration drying
To modified activated carbon.
Adsorb comparative test:
Configuration concentration is 100mg/L lemon yellow solution, and adjusting pH value is 1, weighs the not processed activity of 20mg respectively
The active carbon that charcoal and process the present embodiment are modified is added separately in 500ml100mg/L lemon yellow solution, not processed activity
The adsorption rate of charcoal is 47.7%, is 76% by the modified activated carbon adsorption rate of the present embodiment.
In conjunction with attached drawing, the embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned
Embodiment within the knowledge of a person skilled in the art can also be before not departing from present inventive concept
Put that various changes can be made.
Claims (3)
1. a kind of method of modified activated carbon, it is characterised in that specific step is as follows:
(1) concentrated nitric acid mixing 10 ~ 12h of return stirring is added according to liquid-solid ratio for 100 ~ 150:20 ~ 25ml/g in active carbon first,
It is washed to pH after reaction equal to 7, drying obtains modified product I；
(2) being that 10~15:40~60 are uniformly mixed according to volume ratio by thionyl chloride and DMF obtains mixing organic liquor I, then will
The modified product I that step (1) obtains is that mixing organic liquor I is added at 60~80 DEG C in 50 ~ 75:19 ~ 25ml/g according to liquid-solid ratio
Under the conditions of 10~12h of electromagnetic agitation, filter washed with DMF after reaction, drying obtain modified product II；
(3) being that 10~20:40~50 are uniformly mixed according to volume ratio by ethylenediamine and DMF obtains mixing organic liquor II, then will
Modified product II is that mixing organic liquor II, electromagnetism under conditions of 60~80 DEG C is added in 47 ~ 54:19 ~ 24ml/g according to liquid-solid ratio
10~12h is stirred, washing drying obtains modified product III；
It (4) is that 40~60:4~8:3~6 are mixed according to volume ratio by tetrahydrofuran, triethylamine, chloracetyl chloride
Organic liquor III, the modified product III for then obtaining step (3) are that 45 ~ 50:18 ~ 24ml/g addition mixing is organic according to liquid-solid ratio
Liquid III stirs 10~12h under conditions of 40~50 DEG C, then is dried to obtain modified product IV with tetrahydrofuran wash clean；
(5) modified product IV for obtaining step (4) is that stannous chloride is added in 50 ~ 60:1 ~ 2:2 ~ 4,4,4'- joins according to mass ratio
Pyridine obtains mixture, by vinyl imidazole and DMF according to volume ratio be 5~10:50~70 be uniformly mixed obtain mixing it is organic
Mixing organic liquor IV is added for 50 ~ 55:18 ~ 23ml/g according to liquid-solid ratio, in N in mixture by liquid IV2In atmosphere stirring 24~
Modified activated carbon is prepared after filtration drying in 30h.
2. the method for modified activated carbon according to claim 1, it is characterised in that: concentrated nitric acid concentration in the step (1)
It is 60%~90%.
3. a kind of application for the modified activated carbon that the method for modified activated carbon according to claim 1 or 2 obtains, feature
Be: modified activated carbon application is in adsorpting anion dyestuff process as adsorbent.
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| CN110170315B (en) * | 2019-04-15 | 2021-12-31 | 绍兴文理学院元培学院 | Fiber-based aerogel adsorbent and application thereof in adsorption of dyeing wastewater |
| CN110773127B (en) * | 2019-11-13 | 2021-02-19 | 中国科学院过程工程研究所 | Hydrophobic active carbon material, preparation method and application thereof |
| CN113355154B (en) * | 2021-06-22 | 2023-08-01 | 安徽利民生物科技股份有限公司 | Refining process of peony seed oil |
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| WO2009053972A1 (en) * | 2007-10-22 | 2009-04-30 | Toxsorb Ltd | Modified activated carbon as adsorbent for anionic and cationic inorganic pollutants |
| CN103894160B (en) * | 2014-04-17 | 2015-11-18 | 上海锅炉厂有限公司 | A kind of carbon dioxide solid absorbent and preparation method thereof |
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