[go: up one dir, main page]

CN106865548A - A kind of method that activated carbon is prepared as activator with cobalt acetate and caustic alcohol - Google Patents

A kind of method that activated carbon is prepared as activator with cobalt acetate and caustic alcohol Download PDF

Info

Publication number
CN106865548A
CN106865548A CN201710240503.XA CN201710240503A CN106865548A CN 106865548 A CN106865548 A CN 106865548A CN 201710240503 A CN201710240503 A CN 201710240503A CN 106865548 A CN106865548 A CN 106865548A
Authority
CN
China
Prior art keywords
activated carbon
activator
cobalt acetate
prepared
caustic alcohol
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.)
Pending
Application number
CN201710240503.XA
Other languages
Chinese (zh)
Inventor
冯小旺
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
FUJIAN LIYUAN ACTIVE CARBON INDUSTRIAL Co Ltd
Original Assignee
FUJIAN LIYUAN ACTIVE CARBON INDUSTRIAL Co Ltd
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 FUJIAN LIYUAN ACTIVE CARBON INDUSTRIAL Co Ltd filed Critical FUJIAN LIYUAN ACTIVE CARBON INDUSTRIAL Co Ltd
Priority to CN201710240503.XA priority Critical patent/CN106865548A/en
Publication of CN106865548A publication Critical patent/CN106865548A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/16Pore diameter
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/90Other properties not specified above

Landscapes

  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

It is of the invention to disclose a kind of method that activated carbon is prepared as activator with cobalt acetate and caustic alcohol, belong to method for preparation of active carbon technical field, activated carbon is prepared by activator of organic acid cobalt and caustic alcohol, organic acid cobalt is cobaltous formate or cobalt acetate, it is contemplated that overcoming traditional alkalization method to prepare activated carbon with the inorganic base such as NaOH or potassium hydroxide as activator, compared to organic base, the inorganic base charing of unit mass is inefficient, and the serious shortcoming of the multipair equipment corrosion of consumption, to solve above technical problem, the present invention provides a kind of method that activated carbon is prepared as activator with cobalt acetate and caustic alcohol, by dioxygen water pretreatment, alkalization activation, acidifying is neutralized, it is big that dry four steps obtain aperture, the strong activated carbon of absorption, the inorganic base charing for overcoming unit mass is inefficient, the problem of many high costs of consumption.

Description

A kind of method that activated carbon is prepared as activator with cobalt acetate and caustic alcohol
Technical field
The invention belongs to method for preparation of active carbon technical field, and in particular to one kind is with cobalt acetate and caustic alcohol as activator The method for preparing activated carbon.
Background technology
Activated carbon is that a kind of hole is abundant, specific surface area is big, and physicochemical properties stabilization porous adsorbent, can be effective Organic-inorganic pollutant and heavy metal etc. in ground removal colourity, stink, water.In industrial production, food hygiene, household, transport, ring The numerous areas such as guarantor have pole extensive use.Although the raw material for preparing activated carbon is very extensive, including such as coal, timber, coconut husk, fruit The organic matter rich in carbon such as shell, straw.When being used under some comparing harsh conditions, most of activated carbons are often because of specific surface area Small, adsorption effect is poor, short life the problems such as, cause that charcoal absorption activity failure is fast, change frequent, not only increase and operate into This, also have impact on process continuity.Therefore, exploitation high-adsorption active carbon is always the study hotspot in the field.
Alkali used by traditional alkaline process preparing active carbon is mainly NaOH and potassium hydroxide, on the preparation cost for, With potassium hydroxide price almost, but but there is certain difference on charred effect in the caustic alcohol and NaOH of unit mass It is different, the difference that gained prepares the aspects such as pore size, specific surface area and the life-span of material is mainly reflected in, also, inorganic base is used Amount is more, to consersion unit seriously corroded.
To solve the above problems, such as Chinese patent application(Grant number:CN103877935B)Disclose " strong base anion Acticarbon and its preparation method and application ", it is with alkalescent AC-g-VAm activated carbons as parent, by quaternized anti- Should, the strong alkalinity anion group containing quaternary ammonium group is introduced in activated carbon structure, quaternary ammonium group is:2,3- glycidyl front threes Ammonium chloride or acrylyl oxy-ethyl-trimethyl salmiac.Such adsorbent had both remained the excellent absorption property of activated carbon, together When due to introducing strong base anion cation exchange groups, make such adsorbent that there is sour gas, toxic gas higher clear Except and adsorption efficiency, but quaternary ammonium group class organic compound is somewhat expensive, relatively it is difficult experiment industrialization.
The content of the invention
(1)The technical problem to be solved
The present invention is to activate to overcome traditional alkalization method to prepare activated carbon with the inorganic base such as NaOH or potassium hydroxide Agent, compared to organic base, the inorganic base charing of unit mass is inefficient, and the serious shortcoming of the multipair equipment corrosion of consumption, is Above technical problem is solved, the present invention provides a kind of method that activated carbon is prepared as activator with cobalt acetate and caustic alcohol, with second Sour cobalt doped caustic alcohol is obtained as activator by dioxygen water pretreatment, alkalization activation, acidifying neutralization, dry four steps Aperture is big, adsorb strong activated carbon, and the inorganic base for solving unit mass carbonizes that inefficient, consumption is more, high cost asks Topic.
(2)Technical scheme
In order to solve the above-mentioned technical problem, activity is prepared as activator with cobalt acetate and caustic alcohol the invention provides such a The method of charcoal, activated carbon is prepared by activator of organic acid cobalt and caustic alcohol, and described organic acid cobalt is cobaltous formate or cobalt acetate.
Process includes that dioxygen water pretreatment, alkalization activation, acidifying are neutralized, dried, step specific as follows:
A. dioxygen water pretreatment:Charing raw material is delivered into drying machine to dry to constant weight, drying temperature is no more than 120 DEG C, preferably 100 DEG C, drying is delivered to retort stirring pretreatment 1 ~ 2h, preferably 1.5h after finishing, while it is 3% ~ 10% to be passed through mass fraction Hydrogen peroxide solution, preferably 5% hydrogen peroxide solution, the mass ratio of the hydrogen peroxide solution and the charing raw material is 1:5 ~ 15, Preferred mass ratio is 1:10, reaction temperature is 35 ~ 45 DEG C, preferably 40 DEG C;
B. alkalization activation:The charing raw material adds the pure cobalt acetate of analysis and analysis straight alcohol sodium, cobalt acetate after being cooled to room temperature Quality be the 0.2% ~ 0.5%, preferably 0.3% of the charing raw material, the quality of caustic alcohol is the 3% ~ 5% of the charing raw material, excellent 4% is selected, is sufficiently stirred for, be warming up to 650-750 DEG C, preferably 700 DEG C, heating rate is 5 ~ 8 DEG C/min, preferably 6 DEG C/min, insulation 2 ~ 3h obtains activated material, preferably 2.5h;
C. acidifying is neutralized:Gained activated material and the mixed in hydrochloric acid that mass fraction is 6% ~ 8%, preferably 7% hydrochloric acid, control pH are existed 6.4-6.9, preferably pH are 6.8, are passed through after 10% distilled water to heat and boil, and are cooled to less than 60 DEG C, and preferably 50 DEG C, vacuum is taken out Filter, separation of solid and liquid obtains wet charcoal;
D. dry:The wet charcoal of gained is dried for 400 ~ 500 DEG C in microwave drying furnace, preferably 480 DEG C, programmed rate is 10 ~ 15 DEG C/min, preferably 12 DEG C/min, 400 ~ 500 DEG C of insulations 0.5-1h, preferably 450 DEG C insulation 0.8h in microwave drying furnace, Thoroughly remove moisture and obtain finished product.
(3)Beneficial effect
Beneficial effects of the present invention:
1st, using this faintly acid oxidizing species preprocessing biomass of hydrogen peroxide, cobalt acetate and analysis straight alcohol sodium are recycled Further alkalization obtains function admirable, the carbonized material that aperture is big, specific surface area is high;
2nd, the activated carbon 60min of production is respectively more than 97.8%, more than adsorptive value 1470mg/g to the adsorption rate of methylene blue, And charcoal absorption attenuation rate that this technique productions are obtained is low;
3rd, overcome traditional alkalization method and prepare activated carbon with inorganic base as activator, compared to organic base, unit mass it is inorganic Alkali charing is inefficient, and the serious shortcoming of the multipair equipment corrosion of consumption.
Brief description of the drawings
Fig. 1 is three kinds of embodiments respectively to the effect contrast figure of methylene blue adsorption number.
Specific embodiment
The technical scheme in the embodiment of the present invention is further clearly and completely described with reference to embodiment, is shown So, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.
Embodiment one
In order to solve the above-mentioned technical problem, the present embodiment one provides one kind with cobalt acetate and caustic alcohol as activator prepares activated carbon Method, prepare activated carbon by activator of organic acid cobalt and caustic alcohol, described organic acid cobalt is cobaltous formate or cobalt acetate.
Process includes that dioxygen water pretreatment, alkalization activation, acidifying are neutralized, dried, step specific as follows:
A. dioxygen water pretreatment:Charing raw material is delivered into drying machine to dry to constant weight, drying temperature is 90 DEG C, after drying is finished Retort stirring pretreatment 1h is delivered to, while being passed through the hydrogen peroxide solution that mass fraction is 3%, the hydrogen peroxide solution and institute The mass ratio for stating charing raw material is 1:5, reaction temperature is 35 DEG C;
B. alkalization activation:The charing raw material adds the pure cobalt acetate of analysis and analysis straight alcohol sodium, cobalt acetate after being cooled to room temperature Quality be the 0.2% of the charing raw material, the quality of caustic alcohol is the 3% of the charing raw material, is sufficiently stirred for, and is warming up to 650 DEG C, heating rate is 5 DEG C/min, and insulation 2h obtains activated material;
C. acidifying is neutralized:By the mixed in hydrochloric acid that gained activated material and mass fraction are 6%, pH is 6.4 for control, is passed through 10% distillation Heating is boiled after water, is cooled to less than 40 DEG C, and vacuum filtration, separation of solid and liquid obtains wet charcoal;
D. dry:The wet charcoal of gained is dried for 400 DEG C in microwave drying furnace, programmed rate is 10 DEG C/min, micro- 400 DEG C of insulation 0.5h in ripple drying oven, thoroughly remove moisture and obtain finished product.
Embodiment two
A kind of method that activated carbon is prepared as activator with cobalt acetate and caustic alcohol, with organic acid cobalt and caustic alcohol as activator system Standby activated carbon, described organic acid cobalt is cobaltous formate or cobalt acetate.
Process includes that dioxygen water pretreatment, alkalization activation, acidifying are neutralized, dried, step specific as follows:
A. dioxygen water pretreatment:Charing raw material is delivered into drying machine to dry to constant weight, drying temperature is 100 DEG C, and drying is finished After be delivered to retort stirring pretreatment 1.5h, while being passed through the hydrogen peroxide solution that mass fraction is 5%, the hydrogen peroxide solution Mass ratio with the charing raw material is 1:10, reaction temperature is 40 DEG C;
B. alkalization activation:The charing raw material adds the pure cobalt acetate of analysis and analysis straight alcohol sodium, cobalt acetate after being cooled to room temperature Quality be the 0.3% of the charing raw material, the quality of caustic alcohol is the 4% of the charing raw material, is sufficiently stirred for, and is warming up to 700 DEG C, heating rate is 6 DEG C/min, and insulation 2.5h obtains activated material;
C. acidifying is neutralized:By the mixed in hydrochloric acid that gained activated material and mass fraction are 7%, pH is 6.8 for control, is passed through 10% distillation Heating is boiled after water, is cooled to 50 DEG C, and vacuum filtration, separation of solid and liquid obtains wet charcoal;
D. dry:The wet charcoal of gained is dried for 480 DEG C in microwave drying furnace, programmed rate is 12 DEG C/min, micro- 450 DEG C of insulation 0.8h in ripple drying oven, thoroughly remove moisture and obtain finished product.
Embodiment three
A kind of method that activated carbon is prepared as activator with cobalt acetate and caustic alcohol, with organic acid cobalt and caustic alcohol as activator system Standby activated carbon, described organic acid cobalt is cobaltous formate or cobalt acetate.
Process includes that dioxygen water pretreatment, alkalization activation, acidifying are neutralized, dried, step specific as follows:
A. dioxygen water pretreatment:Charing raw material is delivered into drying machine to dry to constant weight, drying temperature is 120 DEG C, and drying is finished After be delivered to retort stirring pretreatment 2h, while be passed through the hydrogen peroxide solution that mass fraction is 10%, the hydrogen peroxide solution and The mass ratio of the charing raw material is 1:15, reaction temperature is 45 DEG C;
B. alkalization activation:The charing raw material adds the pure cobalt acetate of analysis and analysis straight alcohol sodium, cobalt acetate after being cooled to room temperature Quality be the 0.5% of the charing raw material, the quality of caustic alcohol is the 5% of the charing raw material, is sufficiently stirred for, and is warming up to 750 DEG C, heating rate is 8 DEG C/min, and insulation 3h obtains activated material;
C. acidifying is neutralized:By the mixed in hydrochloric acid that gained activated material and mass fraction are 8%, pH is 6.9 for control, is passed through 10% distillation Heating is boiled after water, is cooled to 60 DEG C, and vacuum filtration, separation of solid and liquid obtains wet charcoal;
D. dry:The wet charcoal of gained is dried for 500 DEG C in microwave drying furnace, programmed rate is 15 DEG C/min, micro- 500 DEG C of insulation 1h in ripple drying oven, thoroughly remove moisture and obtain finished product.
Activated carbon is detected to the adsorptivity of methylene blue in three case study on implementation:
The mg of active carbon finished products 10 weighed in three embodiments is poured into the beaker of 100 mL, and adds 100 mL toward the beaker Methylene blue titer (20 mg/L), opening magnetic stirring apparatus makes composite be in even suspension state.Whole reaction unit It is placed in the camera bellows of lucifuge, and toward logical circulating condensing water in the device, keeps it in 25 ± 1 DEG C.Visible light source is adopted With the iodine-tungsten lamp (PHILIPS Co., launch wavelength >=390 nm) of 150 W, and λ is filtered off with optical filter<The light of 420 nm is ensureing Incident light is entirely visible ray, and the cm of light source distance reaction solution 15, air equably blasts the reaction solution (L/ of throughput 2.5 min).Every 20 min sample 4 mL centrifugations after, take supernatant liquid, measured in ultraviolet-visible spectrophotometer its The absorbance of 665 nm, methylene blue concentration is calculated according to langbobier law, and the degraded of methylene blue is obtained by calculating Rate.
Detected by adsorbing, as shown in figure 1, activated carbon 60min pairs prepared by embodiment one, embodiment two and embodiment three The adsorption rate of methylene blue is respectively 98.5%(1)、99.8%(2)With 97.8%(3), adsorptive value be respectively 1580 ~ 1850mg/g, 1760~2050mg/g、1470~1620mg/g。
Embodiment described above only expresses the preferred embodiment of the present invention, and its description is more specific and detailed, but simultaneously Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art For, without departing from the inventive concept of the premise, some deformations, improvement can also be made and substituted, these belong to this hair Bright protection domain.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.

Claims (3)

1. a kind of method that activated carbon is prepared as activator with cobalt acetate and caustic alcohol, it is characterised in that:With organic acid cobalt and second Sodium alkoxide prepares activated carbon for activator.
2. a kind of method that activated carbon is prepared as activator with cobalt acetate and caustic alcohol according to claim 1, its feature It is:Described organic acid cobalt is cobaltous formate or cobalt acetate.
3. a kind of method that activated carbon is prepared as activator with cobalt acetate and caustic alcohol according to claim 1, technique side Method includes that dioxygen water pretreatment, alkalization activation, acidifying are neutralized, dried, it is characterised in that step specific as follows:
A. dioxygen water pretreatment:Charing raw material is delivered into drying machine to dry to constant weight, drying is delivered to retort and stirs after finishing 1 ~ 2h of pretreatment is mixed, while being passed through the hydrogen peroxide solution that mass fraction is 3% ~ 10%, the hydrogen peroxide solution and the charing are former The mass ratio of material is 1:5 ~ 15, reaction temperature is 35 ~ 45 DEG C;
B. alkalization activation:The charing raw material adds the pure cobalt acetate of analysis and analysis straight alcohol sodium, cobalt acetate after being cooled to room temperature Quality be the 0.2% ~ 0.5% of the charing raw material, the quality of caustic alcohol is the 3% ~ 5% of the charing raw material, is sufficiently stirred for, and is risen To 650-750 DEG C, heating rate is 5 ~ 8 DEG C/min to temperature, and 2 ~ 3h of insulation obtains activated material;
C. acidifying is neutralized:It is 6% ~ 8% mixed in hydrochloric acid by gained activated material and mass fraction, controls pH in 6.4-6.9, is passed through Heating is boiled after 10% distilled water, is cooled to less than 60 DEG C, and vacuum filtration, separation of solid and liquid obtains wet charcoal;
D. dry:The wet charcoal of gained is dried for 400 ~ 500 DEG C in microwave drying furnace, programmed rate be 10 ~ 15 DEG C/ Min, 400 ~ 500 DEG C of insulation 0.5-1h in microwave drying furnace, thoroughly remove moisture and obtain finished product.
CN201710240503.XA 2017-04-13 2017-04-13 A kind of method that activated carbon is prepared as activator with cobalt acetate and caustic alcohol Pending CN106865548A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710240503.XA CN106865548A (en) 2017-04-13 2017-04-13 A kind of method that activated carbon is prepared as activator with cobalt acetate and caustic alcohol

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710240503.XA CN106865548A (en) 2017-04-13 2017-04-13 A kind of method that activated carbon is prepared as activator with cobalt acetate and caustic alcohol

Publications (1)

Publication Number Publication Date
CN106865548A true CN106865548A (en) 2017-06-20

Family

ID=59162178

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710240503.XA Pending CN106865548A (en) 2017-04-13 2017-04-13 A kind of method that activated carbon is prepared as activator with cobalt acetate and caustic alcohol

Country Status (1)

Country Link
CN (1) CN106865548A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111924843A (en) * 2020-08-19 2020-11-13 中国海洋大学 Method for modifying biomass-derived carbon by cyanide and application of method in potassium storage field

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1281383A (en) * 1998-02-10 2001-01-24 康宁股份有限公司 Method for making mesoporous carbon
JP2004216337A (en) * 2003-01-17 2004-08-05 Asahi Kasei Chemicals Corp Method for producing catalyst and epoxy compound
CN103738962A (en) * 2014-01-23 2014-04-23 福建农林大学 Method for preparing active carbon by taking potassium alkoxide as activating agent

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1281383A (en) * 1998-02-10 2001-01-24 康宁股份有限公司 Method for making mesoporous carbon
JP2004216337A (en) * 2003-01-17 2004-08-05 Asahi Kasei Chemicals Corp Method for producing catalyst and epoxy compound
CN103738962A (en) * 2014-01-23 2014-04-23 福建农林大学 Method for preparing active carbon by taking potassium alkoxide as activating agent

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111924843A (en) * 2020-08-19 2020-11-13 中国海洋大学 Method for modifying biomass-derived carbon by cyanide and application of method in potassium storage field

Similar Documents

Publication Publication Date Title
Li et al. Adsorptive Removal of Dyes from Aqueous Solution by KMnO4‐Modified Rice Husk and Rice Straw
CN103949218B (en) A kind of modified graphene adsorbent and preparation method and application
CN109876845B (en) M-g-C3N4Preparation method and application of/rGOA composite adsorption visible light catalytic material
Asrat et al. Adsorption Phenomenon of Arundinaria alpina Stem‐Based Activated Carbon for the Removal of Lead from Aqueous Solution
CN101054176A (en) Granule decoloration active carbon and preparation method thereof
CN101785990A (en) Method for preparing activated carbon-silicon dioxide mixed adsorbing material by using silicon tetrachloride
CN105344319A (en) Preparation method and application of graphene/attapulgite/titanium dioxide composite material
CN109985618B (en) H occupies BiVO4-OVs photocatalytic material, preparation method and application thereof
CN104289188A (en) Preparation of pyromellitic dianhydride modified banana peel adsorbent
CN115779889A (en) A kind of lignin carbon/bismuth molybdate composite photocatalyst and its preparation method and application
CN116603527A (en) Preparation of a biochar-supported cobalt-iron layered double metal oxide catalyst and its application in advanced oxidation
Shang et al. A novel nitrogen heterocyclic ligand-based MOF: synthesis, characterization and photocatalytic properties
CN103482624B (en) Preparation method for active carbon with photocatalysis function
CN105597697A (en) Bamboo charcoal and montmorillonoid composite adsorbent and preparation method thereof
CN108620022B (en) A kind of iodine ion adsorbent, its preparation method and application
CN111440786A (en) Method for removing soil 2,4, 6-trichlorophenol by biomass charcoal immobilized high-efficiency degrading strain
CN112495435A (en) Chitosan-based graphene/TiO2Composite microsphere and preparation method thereof
CN105582902A (en) Composite gel material for treatment of heavy-metal-containing wastewater
CN106311210A (en) A kind of MSn(OH)6 photocatalyst and its preparation method and application
Fu et al. Synthesis and application of wetland plant-based functional materials for aqueous antibiotics removal
Dang et al. Synthesis of nanoporous biochar from rice husk for adsorption of methylene blue
CN106865548A (en) A kind of method that activated carbon is prepared as activator with cobalt acetate and caustic alcohol
Zhang et al. Visible light photocatalytic degradation of oxytetracycline hydrochloride using chitosan-loaded Z-scheme heterostructured material BiOCOOH/O-gC3N4
Wang et al. Reversible controlled switching of photocatalysis for microorganism protection in the coupling of photocatalysis and biodegradation
Hu et al. Removal of ochratoxin A from wine by adsorption-photocatalytic synergy of tubular TiO2/SiO2/g-C3N4: Mechanistic insights and degradation pathways

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20170620

RJ01 Rejection of invention patent application after publication