CN103418341B - Method for preparing activated carbon used for liquid phase adsorption - Google Patents

Method for preparing activated carbon used for liquid phase adsorption Download PDF

Info

Publication number
CN103418341B
CN103418341B CN201310335614.0A CN201310335614A CN103418341B CN 103418341 B CN103418341 B CN 103418341B CN 201310335614 A CN201310335614 A CN 201310335614A CN 103418341 B CN103418341 B CN 103418341B
Authority
CN
China
Prior art keywords
activated carbon
active carbon
liquid phase
magnetic
gel
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201310335614.0A
Other languages
Chinese (zh)
Other versions
CN103418341A (en
Inventor
王新庆
徐靖才
金顶峰
彭晓领
洪波
金红晓
葛洪良
Original Assignee
China Jiliang University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Jiliang University filed Critical China Jiliang University
Priority to CN201310335614.0A priority Critical patent/CN103418341B/en
Publication of CN103418341A publication Critical patent/CN103418341A/en
Application granted granted Critical
Publication of CN103418341B publication Critical patent/CN103418341B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

A method for preparing activated carbon used for liquid phase adsorption relates to a method for preparing magnetic activated carbon. The activated carbon used for liquid phase adsorption is formed by compounding activated carbon and magnetic material, and functional activated carbon can be separated in a liquid phase environment depending on an external magnetic field. The method comprises the following steps: 1, modifying the surfaces of activated carbon particles; 2, taking the activated carbon particles as a carrier, preparing two or more than two metal salt solutions according to a certain proportion, and stirring well; 3, dripping a certain amount of a citric acid complexant, mixing well, dripping ammonia water to regulate the pH of the solution to a certain value, and stirring to form collosol; 4, drying the collosol in certain temperature to form gel; 5, sintering under the protection of nitrogen; 6, magnetically separating, washing and drying. The method has the advantages that the load of a small amount of magnetic material can not influence the adsorption characteristics of activated carbon but can enable the activated carbon to be magnetic, and harmful impurities absorbed under liquid phase condition can be reclaimed and reused through an external magnetic field.

Description

A kind of preparation method of liquid phase adsorption active carbon
Technical field
The present invention relates to a kind of preparation method of magnetic active carbon of liquid phase adsorption.
Background technology
At present in the advanced treating and trade effluent recycling project of Drinking Water; often can encounter and remove the heavy metal ion in former water, organic and inorganic pollution how simply, effectively, economically, reduce the problem such as COD (COD) and peculiar smell in former water.Active carbon is one of adsorbent of extensive use in water treatment absorption method, and it is a kind of charcoal through specially treated, and have countless tiny hole, surface area is huge.The surface area of every gram of active carbon is 500 square metres ~ 1500 square metres.Active carbon has very strong physical absorption and chemisorbed function, but also has detoxication.Detoxication is exactly make use of its huge area, is adsorbed in the micropore of active carbon by poisonous substance, thus stops the absorption of poisonous substance.Active carbon can be combined with number of chemical material simultaneously, thus stops the absorption of these materials.
Active carbon has remarkable characterization of adsorption to Organic substance in water.Because active carbon has flourishing pore structure and huge specific area, therefore to the organic pollution dissolved in water, as benzene-like compounds, phenolic compound, oil and oil product etc. have stronger adsorption capacity, and to the organic pollution being difficult to bioanalysis and other chemical method remove, the organic compound etc. as colourity, foreign odor, methylenum careuleum surface reactive material, herbicide, pesticide, agricultural chemicals, synthetic detergent, synthetic dyestuffs, aminated compounds and many Prof. Du Yucang has good removal effect.Active carbon also has stronger adsorption capacity to some heavy metal compound.As mercury, lead, iron, nickel, chromium, zinc, cobalt etc., therefore, active carbon also has good effect in electroplating wastewater, smelting wastewater process.
Saturated activity charcoal can be reused after regeneration, does not produce secondary pollution.How to reclaim the focus that saturated active carbon in sewage becomes research at present.The present invention relates to a kind of preparation method of magnetic active carbon material, at a small amount of magnetic material of duct internal burden of active carbon, by the effect of external magnetic field, active carbon can be separated from the aqueous solution, ensure the recycling of active carbon Related product.
Summary of the invention
The object of this invention is to provide a kind of magnetic active carbon material and preparation method thereof, at a small amount of magnetic material of duct internal burden of active carbon, by the effect of external magnetic field, active carbon can be separated from the aqueous solution, active carbon and carried magnetic quality of materials are than being 20:(1 ~ 8), can according to external magnetic field strong and weak regulating load amount.
A preparation method for magnetic active carbon material, specifically completes according to the following steps: one, activated carbon powder is broken into activated carbon granule, utilizes 200 mesh sieve screenings; Two, adopt the concentrated sulfuric acid or red fuming nitric acid (RFNA) to carry out surface modification to activated carbon granule, abundant washing (pH=7) is also dry; Three, active carbon, two or more slaine are fully dissolved in deionized water and alcohol mixed solution according to a certain percentage; Four, drip a certain amount of citric acid complexing agent, drip ammoniacal liquor after fully mixing and regulate pH value of solution to certain value, and stir formation colloidal sol; Five, gel is formed by dry at a certain temperature for colloidal sol; Six, gel sinters under nitrogen protection; Seven, through Magneto separate, washing and drying, magnetic-particle supported active Carbon Materials is obtained.
Advantage of the present invention: one, the microstructure of active carbon is not almost destroyed, simple to operate, cost is low; Two, the load of a small amount of magnetic material can not affect the absorption property of active carbon, make active carbon have magnetic simultaneously, can be undertaken extracting or being separated by external magnetic field after charcoal absorption pernicious gas and sewage impurity, be conducive to the recycling realizing active carbon and Related product.
Accompanying drawing explanation
Prepared ferro-cobalt/Conjugate ferrite/absorbent charcoal composite material according to detailed description of the invention 1, wherein Fig. 1 is the XRD collection of illustrative plates of the ferro-cobalt/Conjugate ferrite/active carbon of experiment synthesis; Fig. 2 is the VSM curve of the ferro-cobalt/Conjugate ferrite/active carbon of synthesis; Fig. 3 is magnetic active carbon external magnetic field response condition photo, is magnetic active carbon is placed in alcohol the response condition of observing its external magnetic field in picture.
Detailed description of the invention
Detailed description of the invention 1: first activated carbon powder is broken into activated carbon granule, after utilizing 200 mesh sieve screenings; Adopt the concentrated sulfuric acid to carry out surface modification to activated carbon granule, abundant washing (pH=7) is also dry.Get 4 parts of active carbons, 1 part of Co (NO 3) 26H 2o and 2 part of Fe (NO 3) 39H 2o is dissolved in the mixed solution of 20 parts of ionized waters and 15 parts of alcohol, stirs 2 hours at 60 DEG C of lower magnetic forces.Then dropwise drip 0.5 part of citric acid as complexing agent, drip ammoniacal liquor after stirring 5h and regulate pH value of solution=3, regulate bath temperature to 70 DEG C, being stirred to solution becomes collosol state.Gained colloidal sol to be transferred in air dry oven dry 3h at 250 DEG C, obtain gel.Under nitrogen protection, gel is placed in 700 DEG C, tube furnace sintering 3h.Through Magneto separate, washing (pH=7) and drying, obtain magnetic-particle supported active Carbon Materials.
Detailed description of the invention 2: first activated carbon powder is broken into activated carbon granule, after utilizing 200 mesh sieve screenings; Adopt the concentrated sulfuric acid to carry out surface modification to activated carbon granule, abundant washing (pH=7) is also dry.Get 4 parts of active carbons, 1 part of MnCl 26H 2o and 2 part of Fe (NO 3) 39H 2o is dissolved in the mixed solution of 20 parts of ionized waters and 15 parts of alcohol, stirs 2 hours at 60 DEG C of lower magnetic forces.Then dropwise drip 2 parts of citric acids as complexing agent, drip ammoniacal liquor after stirring 5h and regulate pH value of solution=5, regulate bath temperature to 70 DEG C, being stirred to solution becomes collosol state.Gained colloidal sol to be transferred in air dry oven dry 3h at 250 DEG C, obtain gel.Under nitrogen protection, gel is placed in 500 DEG C, tube furnace sintering 3h.Through Magneto separate, washing (pH=7) and drying, obtain magnetic-particle supported active Carbon Materials.
Detailed description of the invention 3: first activated carbon powder is broken into activated carbon granule, after utilizing 200 mesh sieve screenings; Adopt red fuming nitric acid (RFNA) to carry out surface modification to activated carbon granule, abundant washing (pH=7) is also dry.Get 4 parts of active carbons, 1 part of Zn (NO 3) 26H 2o and 2 part of Fe (NO 3) 39H 2o is dissolved in the mixed solution of 20 parts of ionized waters and 15 parts of alcohol, stirs 2 hours at 60 DEG C of lower magnetic forces.Then dropwise drip 2 parts of citric acids as complexing agent, drip ammoniacal liquor after stirring 5h and regulate pH value of solution=7, regulate bath temperature to 70 DEG C, being stirred to solution becomes collosol state.Gained colloidal sol to be transferred in air dry oven dry 3h at 250 DEG C, obtain gel.Under nitrogen protection, gel is placed in 500 DEG C, tube furnace sintering 3h.Through Magneto separate, washing (pH=7) and drying, obtain magnetic-particle supported active Carbon Materials.
Detailed description of the invention 4: first activated carbon powder is broken into activated carbon granule, after utilizing 200 mesh sieve screenings; Adopt the concentrated sulfuric acid to carry out surface modification to activated carbon granule, abundant washing (pH=7) is also dry.Get 4 parts of active carbons, 0.5 part of MnCl 26H 2o, 0.5 part of ZnCl 26H 2o and 2 part of Fe (NO 3) 39H 2o is dissolved in the mixed solution of 20 parts of ionized waters and 15 parts of alcohol, stirs 2 hours at 60 DEG C of lower magnetic forces.Then dropwise drip 3 parts of citric acids as complexing agent, drip ammoniacal liquor after stirring 5h and regulate pH value of solution=7, regulate bath temperature to 70 DEG C, being stirred to solution becomes collosol state.Gained colloidal sol to be transferred in air dry oven dry 3h at 250 DEG C, obtain gel.Under nitrogen protection, gel is placed in 700 DEG C, tube furnace sintering 3h.Through Magneto separate, washing (pH=7) and drying, obtain magnetic-particle supported active Carbon Materials.
Detailed description of the invention 5: first activated carbon powder is broken into activated carbon granule, after utilizing 200 mesh sieve screenings; Adopt the concentrated sulfuric acid to carry out surface modification to activated carbon granule, abundant washing (pH=7) is also dry.Get 4 parts of active carbons, 0.5 part of NiCl 26H 2o, 0.5 part of Zn (NO 3) 26H 2o and 2 part of Fe (NO 3) 39H 2o is dissolved in the mixed solution of 20 parts of ionized waters and 15 parts of alcohol, stirs 2 hours at 60 DEG C of lower magnetic forces.Then dropwise drip 3 parts of citric acids as complexing agent, drip ammoniacal liquor after stirring 5h and regulate pH value of solution=7, regulate bath temperature to 70 DEG C, being stirred to solution becomes collosol state.Gained colloidal sol to be transferred in air dry oven dry 3h at 250 DEG C, obtain gel.Under nitrogen protection, gel is placed in 700 DEG C, tube furnace sintering 3h.Through Magneto separate, washing (pH=7) and drying, obtain magnetic-particle supported active Carbon Materials.
Detailed description of the invention 6: first activated carbon powder is broken into activated carbon granule, after utilizing 200 mesh sieve screenings; Adopt the concentrated sulfuric acid to carry out surface modification to activated carbon granule, abundant washing (pH=7) is also dry.Get 30 parts of active carbons, 1 part of BaCl 26H 2o and 12 part of Fe (NO 3) 39H 2o is dissolved in the mixed solution of 20 parts of ionized waters and 15 parts of alcohol, stirs 2 hours at 60 DEG C of lower magnetic forces.Then dropwise drip 24 parts of citric acids as complexing agent, drip ammoniacal liquor after stirring 5h and regulate pH value of solution=7, regulate bath temperature to 70 DEG C, being stirred to solution becomes collosol state.Gained colloidal sol to be transferred in air dry oven dry 3h at 250 DEG C, obtain gel.Under nitrogen protection, gel is placed in 700 DEG C, tube furnace sintering 3h.Through Magneto separate, washing (pH=7) and drying, obtain magnetic-particle supported active Carbon Materials.
Detailed description of the invention 7: first activated carbon powder is broken into activated carbon granule, after utilizing 200 mesh sieve screenings; Adopt the concentrated sulfuric acid to carry out surface modification to activated carbon granule, abundant washing (pH=7) is also dry.Get 4 parts of active carbons, 1 part of Cu (NO 3) 23H 2o and 2 part of Fe (NO 3) 39H 2o is dissolved in the mixed solution of 20 parts of ionized waters and 15 parts of alcohol, stirs 2 hours at 60 DEG C of lower magnetic forces.Then dropwise drip 4 parts of citric acids as complexing agent, drip ammoniacal liquor after stirring 5h and regulate pH value of solution=7, regulate bath temperature to 70 DEG C, being stirred to solution becomes collosol state.Gained colloidal sol to be transferred in air dry oven dry 3h at 250 DEG C, obtain gel.Under nitrogen protection, gel is placed in 700 DEG C, tube furnace sintering 3h.Through Magneto separate, washing (pH=7) and drying, obtain magnetic-particle supported active Carbon Materials.
Detailed description of the invention 8: first activated carbon powder is broken into activated carbon granule, after utilizing 200 mesh sieve screenings; Adopt the concentrated sulfuric acid to carry out surface modification to activated carbon granule, abundant washing (pH=7) is also dry.Get 4 parts of active carbons, 0.5 part of Cu (NO 3) 23H 2o, 0.5 part of Zn (NO 3) 26H 2o and 2 part of Fe (NO 3) 39H 2o is dissolved in the mixed solution of 20 parts of ionized waters and 15 parts of alcohol, stirs 2 hours at 60 DEG C of lower magnetic forces.Then dropwise drip 4 parts of citric acids as complexing agent, drip ammoniacal liquor after stirring 5h and regulate pH value of solution=4, regulate bath temperature to 70 DEG C, being stirred to solution becomes collosol state.Gained colloidal sol to be transferred in air dry oven dry 3h at 250 DEG C, obtain gel.Under nitrogen protection, gel is placed in 700 DEG C, tube furnace sintering 3h.Through Magneto separate, washing (pH=7) and drying, obtain magnetic-particle supported active Carbon Materials.

Claims (2)

1. the preparation method of a liquid phase adsorption active carbon, it is characterized in that the duct internal burden magnetic-particle at active carbon, its preparation method adopts sol-gel process synthesis, concrete steps are as follows: one, adopt the concentrated sulfuric acid or red fuming nitric acid (RFNA) to carry out surface modification to activated carbon granule, fully washing is also dry; Two, active carbon and two kinds or more slaine is fully dissolved in deionized water and alcohol mixed solution according to a certain percentage; Three, drip citric acid complexing agent, citric acid and total metal ion mol ratio are 0.5 ~ 4, drip ammoniacal liquor and regulate pH value of solution to 4 ~ 7 after fully mixing, and stir formation colloidal sol; Four, gel is formed by dry at 120 DEG C ~ 250 DEG C for colloidal sol; Five, gel 400 DEG C under nitrogen protection ~ 800 DEG C sintering 1 ~ 3h; Six, through Magneto separate, washing and drying, a kind of liquid phase adsorption active carbon is obtained.
2. the preparation method of a kind of liquid phase adsorption active carbon according to claim 1, is characterized in that: the slaine of employing is chloride, nitrate and sulfate, and metal ion is Ni 2+, Fe 2+, Co 2+, Mn 2+, Ba 2+, Zn 2+, Cu 2+.
CN201310335614.0A 2013-08-03 2013-08-03 Method for preparing activated carbon used for liquid phase adsorption Active CN103418341B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310335614.0A CN103418341B (en) 2013-08-03 2013-08-03 Method for preparing activated carbon used for liquid phase adsorption

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310335614.0A CN103418341B (en) 2013-08-03 2013-08-03 Method for preparing activated carbon used for liquid phase adsorption

Publications (2)

Publication Number Publication Date
CN103418341A CN103418341A (en) 2013-12-04
CN103418341B true CN103418341B (en) 2015-06-17

Family

ID=49644027

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310335614.0A Active CN103418341B (en) 2013-08-03 2013-08-03 Method for preparing activated carbon used for liquid phase adsorption

Country Status (1)

Country Link
CN (1) CN103418341B (en)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107551673A (en) * 2017-08-10 2018-01-09 深圳沃海森科技有限公司 Antibacterial filter core used for automobile air conditioning and its preparation technology
CN109731550A (en) * 2019-03-21 2019-05-10 中国计量大学 It is a kind of can Magneto separate absorbent charcoal composite material preparation method
CN110233060B (en) * 2019-04-30 2021-06-22 杭州星宇炭素环保科技有限公司 Active carbon metal oxide electrode material and its synthesis process
CN110302800B (en) * 2019-04-30 2022-03-11 杭州星宇炭素环保科技有限公司 Synthesis process of catalyst activated carbon composite material for decomposing dioxin

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101475367A (en) * 2009-01-22 2009-07-08 中国计量学院 Preparation of nanometer-level barium ferrite magnetic material
CN101683624A (en) * 2008-09-27 2010-03-31 中国科学院大连化学物理研究所 Control method for carrying metal particles in carbon nanotube cavity or on external wall

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101683624A (en) * 2008-09-27 2010-03-31 中国科学院大连化学物理研究所 Control method for carrying metal particles in carbon nanotube cavity or on external wall
CN101475367A (en) * 2009-01-22 2009-07-08 中国计量学院 Preparation of nanometer-level barium ferrite magnetic material

Also Published As

Publication number Publication date
CN103418341A (en) 2013-12-04

Similar Documents

Publication Publication Date Title
Li et al. Removal of phosphate from aqueous solution by dolomite-modified biochar derived from urban dewatered sewage sludge
Liu et al. Resource utilization of swine sludge to prepare modified biochar adsorbent for the efficient removal of Pb (II) from water
Wang et al. Highly effective remediation of Pb (II) and Hg (II) contaminated wastewater and soil by flower-like magnetic MoS2 nanohybrid
Cui et al. Phosphorus recovery by core-shell γ-Al2O3/Fe3O4 biochar composite from aqueous phosphate solutions
Shan et al. Remarkable phosphate removal and recovery from wastewater by magnetically recyclable La2O2CO3/γ-Fe2O3 nanocomposites
Yang et al. Adsorption of Sb (III) from aqueous solution by QFGO particles in batch and fixed-bed systems
Tu et al. Phosphorus adsorption onto green synthesized nano-bimetal ferrites: equilibrium, kinetic and thermodynamic investigation
CN103506065B (en) A kind of Magnetic heavy metal adsorbent with casing-core structure and preparation method thereof
Ji et al. Sorption enhancement of nickel (II) from wastewater by ZIF-8 modified with poly (sodium 4-styrenesulfonate): Mechanism and kinetic study
CN103418341B (en) Method for preparing activated carbon used for liquid phase adsorption
CN106861615A (en) A kind of charcoal magnetic Fe3S4Composite nano adsorbent and preparation method and application
CN103007881A (en) Magnetically separated bamboo charcoal-based wastewater treatment agent and preparation method and application thereof
Liao et al. The construction of magnetic hydroxyapatite-functionalized pig manure-derived biochar for the efficient uranium separation
CN109499523A (en) A kind of FeOOH/MnO2The preparation method of@diatomite composite material
CN103418342A (en) Preparation method of magnetically-separable active carbon material
CN104353437A (en) Core-shell magnetic poly(m-phenylene diamine) nano-particle, preparation method and application thereof
Huang et al. In situ decoration of La (OH) 3 on polyethyleneimine-linked dendritic mesoporous silica nanospheres targeting at efficient and simultaneous removal of phosphate and Congo red
CN106268617A (en) Fe2O3 doping manganese dioxide micro-nano structure material and preparation method and application
Wang et al. Cr (VI) Removal from Aqueous Solution Using Starch and Sodium Carboxymethyl Cellulose-Coated Fe and Fe/Ni Nanoparticles.
Gao et al. Removal of cadmium (II) from aqueous solutions by a novel sulfide-modified nanoscale zero-valent iron supported on kaolinite: Treatment efficiency, kinetics and mechanisms
CN105439272A (en) Method for applying ferrite MFe2O4 magnetic nano-particles to removal of tellurium-containing wastewater and application of ferrite MFe2O4 magnetic nano-particles
CN102531094B (en) Treatment method of wastewater containing heavy metal ions or phosphorus
CN111905702A (en) Preparation method of porous particle filter material loaded with nano zero-valent iron for adsorbing and removing heavy metals in water
Wang et al. Investigation on the room-temperature preparation and application of chain-like iron flower and its ramifications in wastewater purification
CN107362776B (en) Sulfobetaine and inorganic salt composite modified clay, preparation method and application thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
ASS Succession or assignment of patent right

Owner name: CHINA JILIANG UNIVERSITY

Free format text: FORMER OWNER: PENG XIAOLING

Effective date: 20150515

C41 Transfer of patent application or patent right or utility model
TA01 Transfer of patent application right

Effective date of registration: 20150515

Address after: Hangzhou City, Zhejiang province 310018 Jianggan District Xiasha Higher Education Park source Street No. 258

Applicant after: China Jiliang University

Address before: Hangzhou City, Zhejiang province 311112 ancient Pier Road, Yuhang District Ming Nga East 15-1-101

Applicant before: Peng Xiaoling

C14 Grant of patent or utility model
GR01 Patent grant
CP03 Change of name, title or address

Address after: 310018 China Metrology University, 258 Xiasha Xueyuan Street, Hangzhou City, Zhejiang Province

Patentee after: CHINA JILIANG UNIVERSITY

Address before: 310018 No. 258, Xue Yuan Street, Xiasha Higher Education Park, Jianggan District, Hangzhou, Zhejiang.

Patentee before: China Jiliang University

CP03 Change of name, title or address
EE01 Entry into force of recordation of patent licensing contract
EE01 Entry into force of recordation of patent licensing contract

Application publication date: 20131204

Assignee: HANGZHOU XINGYU CARBON TECHNOLOGY GREEN Co.,Ltd.

Assignor: China Jiliang University

Contract record no.: X2020980006148

Denomination of invention: A preparation method of activated carbon for liquid phase adsorption

Granted publication date: 20150617

License type: Exclusive License

Record date: 20200917