CN109174005A - A kind of method of modifying of regenerated carbon - Google Patents

A kind of method of modifying of regenerated carbon Download PDF

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Publication number
CN109174005A
CN109174005A CN201811318084.8A CN201811318084A CN109174005A CN 109174005 A CN109174005 A CN 109174005A CN 201811318084 A CN201811318084 A CN 201811318084A CN 109174005 A CN109174005 A CN 109174005A
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CN
China
Prior art keywords
regenerated carbon
filter cake
modifying
regenerated
concentration
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Pending
Application number
CN201811318084.8A
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Chinese (zh)
Inventor
刘程
刘洪杰
苏云瑞
刘少杰
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Hebei University of Science and Technology
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Hebei University of Science and Technology
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Priority to CN201811318084.8A priority Critical patent/CN109174005A/en
Publication of CN109174005A publication Critical patent/CN109174005A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/283Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen

Abstract

The present invention relates to a kind of method of modifying of regenerated carbon, specifically: (1) room temperature under, regenerated carbon is put into reaction kettle, is added after aqueous nitrogen Fertilizer solution is sufficiently mixed and stands;(2) by the material filtering in step (1), filter cake be washed with water after in 105 DEG C of dryings;(3) filter cake after drying in step (2) is modified at 500 DEG C~700 DEG C 2~5h, obtains modified regenerated carbon after cooling.The method improve the pore structure of regenerated carbon and chemical property, improve the adsorption capacity of regenerated carbon, solve the problems, such as that regenerated carbon methylene blue adsorption value is relatively low;Have the characteristics that raw material sources are wide, price is low, easy to operate, modified effect is obvious.

Description

A kind of method of modifying of regenerated carbon
Technical field
The present invention relates to a kind of method of modifying of regenerated carbon, in particular to for adsorbing methylene blue in sewage treatment Regenerated carbon method of modifying.
Background technique
Methylene blue is a kind of basic dye for being usually used in the substance stains such as cotton, timber and silk, and Acute exposure can be led Cause human heart rate's quickening, vomiting, shock etc..Since methylene blue has high chroma, water can be made under lower concentration Blue is presented to influence water quality, it is therefore desirable to be handled before discharge of wastewater.
The dyestuff that active carbon is used to handle in waste water can obtain preferable effect.Since the production cost of active carbon is higher, Hot recycling usually industrially is carried out to the active carbon for losing absorption property after using.And regenerative process can cause activated carbon capillary hole Road collapses, Carbon deposition blocks duct etc., will lead to the decline of regenerated carbon absorption property.In addition, there are ash content height, hole for active carbon The limitation for holding the disadvantages of small, micropore distribution is wide and adsorptive selectivity can be poor and surface functional group and electrochemical properties, causes Its adsorption efficiency and adsorption capacity are lower.In order to improve the methylene blue adsorption number performance of regenerated carbon, need to regeneration activity Charcoal is modified.
The present invention provides a kind of method of modifying for the regenerated carbon of processing basic dye methylene blue waste water.It should Method is used as modifying agent using nitrogenous fertilizer (ammonium chloride, ammonium sulfate and urea), by the modified pore structure for adjusting regenerated carbon And distribution, and increase the content of its surface acidity functional group, to increase the active adsorption sites of regenerated carbon, reach increasing Add the purpose of the absorption property of regenerated carbon.
Summary of the invention
In view of the above-mentioned problems, the present invention provides a kind of method of modifying of regenerated carbon, by control material proportion and Regenerated carbon after processing waste water from dyestuff is passed through and the technical process such as impregnates, washes and be modified by modifying technology conditions, and raising is again The absorption property of liveliness proof charcoal.
A kind of method of modifying of regenerated carbon, the specific steps are as follows:
(1) it impregnates: at normal temperature, 20 parts of regenerated carbons being put into reaction kettle, it is 100g/L that 80~100 parts of concentration, which are added, The nitrogenous fertilizer modifier aqueous solution of~250g/L stands 16~24 hours after being sufficiently mixed.
(2) wash: by the material filtering in step (1), filter cake be washed with water after in 105 DEG C of dryings.
(3) modified: the filter cake after drying in step (2) being modified 2~5h at 500 DEG C~700 DEG C, is changed after cooling The regenerated carbon of property.
Preferably: nitrogenous fertilizer modifying agent is ammonium sulfate, ammonium chloride or urea in step (1).
Preferably: the concentration of ammonium sulfate is 100g/L in step (1), the concentration of ammonium chloride is 100g/L or the concentration of urea For 200g/L;Modification temperature in step (3) is 600 DEG C, modification time 3h.
The invention has the following beneficial effects: (1), the present invention selects nitrogenous fertilizer as modifying agent, increases regenerated carbon Microvoid content and micropore surface carboxyl functional group quantity, improve the pore structure and chemical property of regenerated carbon, improve The adsorption capacity of regenerated carbon solves the problems, such as that regenerated carbon methylene blue adsorption value is relatively low, again for waste active carbon It makes profits with offer technical support;(2) this method has the spies such as raw material sources are wide, price is low, easy to operate, modified effect is obvious Point;(3) this method is remained without modifying agent, and new pollution will not be generated to treating material, is a kind of environmentally protective modification side Method.
Specific embodiment
Below with reference to embodiment, the invention will be further described.Regenerated carbon used in embodiment, modification regeneration Active carbon passes through 200 mesh sieve;The methylene blue adsorption value of unmodified regenerated carbon is 293.1mg/g, methylene blue adsorption value Measurement using the method in GB/T 12496.10-1999.
Embodiment 1
(1) at room temperature, 20g regenerated carbon, the ammonium sulfate solution that 100g concentration is 100g/L are placed in conical flask, are stirred 20h is stood after being sufficiently mixed within 30 minutes.
(2) material filtering in step (1) is put into air dry oven after filter cake washs 2 times with 120mL deionized water In dry 4 hours at 105 DEG C.
(3) filter cake of step (2) after dry is put into tube furnace, constant temperature 3 hours, natural cooling after being warming up to 650 DEG C It is taken out after to 100 DEG C, obtains modification regeneration active carbon, measuring its methylene blue adsorption value is 373.2mg/g, improves 27.3%.
Use N2The pore appearance that adsorption isotherm and BJH model measure 2~4nm in modification regeneration active carbon increases 16%;Using Boehm titration determination modification regeneration activated carbon capillary surface carboxyl groups, functional group increases 80%, this is all to improve its suction The reason of attached ability.
Embodiment 2
(1) at room temperature, 20g regenerated carbon, the ammonium sulfate solution that 95g concentration is 150g/L are placed in conical flask, are stirred It is stood for 24 hours after being sufficiently mixed within 30 minutes.
(2) by the material filtering in step (1), filter cake is washed 2 times using 120mL deionized water, is put into air dry oven In dry 4 hours at 105 DEG C.
(3) filter cake of step (2) after dry is put into tube furnace, constant temperature 5 hours, natural cooling after being warming up to 700 DEG C It is taken out after to 100 DEG C, obtains modification regeneration active carbon, measuring its methylene blue adsorption value is 355.3mg/g, increases 21.2%.
Embodiment 3
(1) at room temperature, 20g regenerated carbon, the ammonium sulfate solution that 80g concentration is 200g/L are placed in conical flask, are stirred 22h is stood after being sufficiently mixed within 30 minutes.
(2) step (1) is stood gained charcoal liquid to filter, filter cake is washed 2 times using 120mL deionized water, and it is dry to be put into air blast It is 4 hours dry at 105 DEG C in dry case.
(3) filter cake of step (2) after dry is put into tube furnace, constant temperature 4 hours, natural cooling after being warming up to 500 DEG C It is taken out after to 100 DEG C, obtains modification regeneration active carbon, measuring its methylene blue adsorption value is 346.3mg/g, increases 18.1%.
Embodiment 4
(1) at room temperature, 20g regenerated carbon, the ammonium sulfate solution that 90g concentration is 250g/L are placed in conical flask, are stirred 16h is stood after being sufficiently mixed within 30 minutes.
(2) step (1) is stood gained charcoal liquid to filter, filter cake is washed 2 times using 120mL deionized water, and it is dry to be put into air blast It is 4 hours dry at 105 DEG C in dry case.
(3) filter cake of step (2) after dry is put into tube furnace, constant temperature 2 hours, natural cooling after being warming up to 550 DEG C It is taken out after to 100 DEG C, obtains modification regeneration active carbon, measuring its methylene blue adsorption value is 331.6mg/g, increases 13.1%.
Embodiment 5
(1) at room temperature, 20g regenerated carbon, the aqueous ammonium chloride solution that 100g concentration is 100g/L are placed in conical flask, are stirred 20h is stood after being sufficiently mixed within 30 minutes.
(2) by the material filtering in step (1), filter cake is washed 2 times using 120mL deionized water, is put into air dry oven In dry 4 hours at 105 DEG C.
(3) filter cake of step (2) after dry is put into tube furnace, constant temperature 3 hours, natural cooling after being warming up to 700 DEG C It is taken out after to 100 DEG C, obtains modification regeneration active carbon, measuring its adsorptive value is 363.5mg/g, improves 24.0%.
Embodiment 6
(1) at room temperature, 20g regenerated carbon, the aqueous ammonium chloride solution that 95g concentration is 150g/L are placed in conical flask, are stirred It is stood for 24 hours after being sufficiently mixed within 30 minutes.
(2) by the material filtering in step (1), filter cake is washed 2 times using 120mL deionized water, is put into air dry oven In dry 4 hours at 105 DEG C.
(3) filter cake of step (2) after dry is put into tube furnace, constant temperature 5 hours, natural cooling after being warming up to 650 DEG C It is taken out after to 100 DEG C, obtains modification regeneration active carbon, measuring its adsorptive value is 357.4mg/g, improves 21.9%.
Embodiment 7
(1) at room temperature, 20g regenerated carbon, the aqueous ammonium chloride solution that 80g concentration is 200g/L are placed in conical flask, are stirred 22h is stood after being sufficiently mixed within 30 minutes.
(2) by the material filtering in step (1), filter cake is washed 2 times using 120mL deionized water, is put into air dry oven In dry 4 hours at 105 DEG C.
(3) filter cake of step (2) after dry is put into tube furnace, constant temperature 4 hours, natural cooling after being warming up to 550 DEG C It is taken out after to 100 DEG C, obtains modification regeneration active carbon, measuring its adsorptive value is 356.5mg/g, improves 21.6%.
Embodiment 8
(1) at room temperature, 20g regenerated carbon, the aqueous ammonium chloride solution that 90g concentration is 250g/L are placed in conical flask, are stirred 16h is stood after being sufficiently mixed within 30 minutes.
(2) by the material filtering in step (1), filter cake is washed 2 times using 120mL deionized water, is put into air dry oven In dry 4 hours at 105 DEG C.
(3) filter cake of step (2) after dry is put into tube furnace, constant temperature 2 hours, natural cooling after being warming up to 500 DEG C It is taken out after to 100 DEG C, obtains modification regeneration active carbon, measuring its adsorptive value is 348.7mg/g, improves 19.0%.
Embodiment 9
(1) at room temperature, 20g regenerated carbon, the aqueous solution of urea that 100g concentration is 200g/L are placed in conical flask, stirring 30 Minute stands 20h after being sufficiently mixed.
(2) by the material filtering in step (1), filter cake is washed 2 times using 120mL deionized water, is put into air dry oven In dry 4 hours at 105 DEG C.
(3) filter cake of step (2) after dry is put into tube furnace, constant temperature 4 hours, natural cooling after being warming up to 600 DEG C It is taken out after to 100 DEG C, obtains modification regeneration active carbon, measuring its adsorptive value is 338.3mg/g, improves 15.4%.
Embodiment 10
(1) at room temperature, 20g regenerated carbon, the aqueous solution of urea that 95g concentration is 150g/L are placed in conical flask, stirring 30 Minute stands for 24 hours after being sufficiently mixed.
(2) by the material filtering in step (1), filter cake is washed 2 times using 120mL deionized water, is put into air dry oven In dry 4 hours at 105 DEG C.
(3) filter cake of step (2) after dry is put into tube furnace, constant temperature 5 hours, natural cooling after being warming up to 500 DEG C It is taken out after to 100 DEG C, obtains modification regeneration active carbon, measuring its adsorptive value is 341.6mg/g, improves 16.5%.
Embodiment 11
(1) at room temperature, 20g regenerated carbon, the aqueous solution of urea that 80g concentration is 200g/L are placed in conical flask, stirring 30 Minute stands 22h after being sufficiently mixed.
(2) by the material filtering in step (1), filter cake is washed 2 times using 120mL deionized water, is put into air dry oven In dry 3 hours at 105 DEG C.
(3) filter cake of step (2) after dry is put into tube furnace, constant temperature 3 hours, natural cooling after being warming up to 650 DEG C It is taken out after to 100 DEG C, obtains modification regeneration active carbon, measuring its adsorptive value is 355.2mg/g, improves 21.1%.
Embodiment 12
(1) at room temperature, 20g regenerated carbon, the aqueous solution of urea that 90g concentration is 250g/L are placed in conical flask, stirring 30 Minute stands 16h after being sufficiently mixed.
(2) by the material filtering in step (1), filter cake is washed 2 times using 120mL deionized water, is put into air dry oven In dry 4 hours at 105 DEG C.
(3) filter cake of step (2) after dry is put into tube furnace, constant temperature 2 hours, natural cooling after being warming up to 700 DEG C It is taken out after to 100 DEG C, obtains modification regeneration active carbon, measuring its adsorptive value is 342.8mg/g, improves 17.0%.

Claims (3)

1. a kind of method of modifying of regenerated carbon, it is characterised in that comprise the steps of:
(1) it impregnates: at normal temperature, 20 parts of regenerated carbons being put into reaction kettle, it is 100g/L that 80~100 parts of concentration, which are added, The nitrogenous fertilizer modifier aqueous solution of~250g/L stands 16~24 hours after being sufficiently mixed;
(2) wash: by the material filtering in step (1), filter cake be washed with water after in 105 DEG C of dryings;
(3) modified: the filter cake after drying in step (2) being modified 2~5h at 500 DEG C~700 DEG C, modification is obtained after cooling Regenerated carbon.
2. a kind of method of modifying of regenerated carbon according to claim 1, it is characterised in that: in the step (1) Nitrogenous fertilizer modifying agent is ammonium sulfate, ammonium chloride or urea.
3. a kind of method of modifying of regenerated carbon according to claim 2, it is characterised in that: in the step (1) The concentration of ammonium sulfate is 100g/L, the concentration of ammonium chloride is 100g/L or the concentration of urea is 200g/L;Modification in step (3) Temperature is 600 DEG C, modification time 3h.
CN201811318084.8A 2018-11-07 2018-11-07 A kind of method of modifying of regenerated carbon Pending CN109174005A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102921473A (en) * 2012-09-28 2013-02-13 石河子大学 Novel nitrogen-modified carbon catalyst carrier and preparation method and use thereof
CN103372418A (en) * 2012-04-28 2013-10-30 东南大学 Modified activated carbon demercuration adsorbent and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103372418A (en) * 2012-04-28 2013-10-30 东南大学 Modified activated carbon demercuration adsorbent and preparation method thereof
CN102921473A (en) * 2012-09-28 2013-02-13 石河子大学 Novel nitrogen-modified carbon catalyst carrier and preparation method and use thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
肖榕: ""尿素改性活性炭对水中汞离子的吸附性能研究"", 《广州化工》 *
贾瑛等: "《轻质碳材料的应用》", 30 November 2013 *

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Application publication date: 20190111