CN106807327A - A kind of load Nanoscale Iron bentone adsorbent sterilized for metallurgical briquetting zinc ion and preparation method thereof - Google Patents

A kind of load Nanoscale Iron bentone adsorbent sterilized for metallurgical briquetting zinc ion and preparation method thereof Download PDF

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CN106807327A
CN106807327A CN201611198510.XA CN201611198510A CN106807327A CN 106807327 A CN106807327 A CN 106807327A CN 201611198510 A CN201611198510 A CN 201611198510A CN 106807327 A CN106807327 A CN 106807327A
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solution
sterilized
zinc ion
activated carbon
ethanol
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罗彦保
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Peng Lei New Material Co Ltd Of Wuhu City
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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
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12—Naturally occurring clays or bleaching earth
    • 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
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/024—Compounds of Zn, Cd, Hg
    • B01J20/0244—Compounds of Zn
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
    • B01J20/0281—Sulfates of compounds other than those provided for in B01J20/045
    • 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
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
    • B01J23/8906—Iron and noble metals
    • 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
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • 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
    • C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
    • 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
    • C02F1/70—Treatment of water, waste water, or sewage by reduction
    • C02F1/705—Reduction by metals
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • 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
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C02F2101/22—Chromium or chromium compounds, e.g. chromates
    • 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
    • C02F2103/06—Contaminated groundwater or leachate

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Abstract

The invention discloses a kind of load Nanoscale Iron bentone adsorbent sterilized for metallurgical briquetting zinc ion and preparation method thereof, it is characterised in that be made up of the raw material of following weight portion：Attapulgite 35, sodium bentonite 30 50, activated carbon 5 10, hydrochloric acid solution 36, silver nitrate solution 10 15, FeSO4·7H2O 10 20, solution of zinc sulfate 37, KBH4 5 10, NaOH 20 30, deoxidation appropriate amount of water, deionized water 30 80, deoxygenated ethanol 20 100, ethanol 20 40；Present invention introduces active carbon loading silver, on the one hand can increase bentonitic specific surface area, so as to increase the contact area of adsorbent and pollutant, improve adsorption efficiency；Another aspect silver particles can activate the nanometer iron catalyst for having inactivated, and catalysis activity, clean-up effect be improved, while increasing the service life；Coordinating the zinc ion of addition has sterilized and anti-detonation.

Description

A kind of load Nanoscale Iron bentone adsorbent sterilized for metallurgical briquetting zinc ion and Its preparation method
Technical field
The invention belongs to ground water cleaning field, and in particular to a kind of load nanometer sterilized for metallurgical briquetting zinc ion Iron bentone adsorbent and preparation method thereof.
Background technology
Bentonite is the natural nano sorbing material with montmorillonite as main component, and cation exchange capacity is big, to pollution Thing has stronger adsorption capacity, and the adsorption treatment of Industry Waste organic pollutants, heavy metal is widely used in recent years. Additionally, bentonite is also widely used for the fields such as oil, daily, chemical industry, the energy and environmental protection.Nanoscale Iron is compared to common iron Grain, activity is high, and clean effect is fast.In recent years, heavy metal in underground water is hexavalent chromium polluted to be increasingly subject to pay attention to, and Nanoscale Iron can be with Effectively by hexavalent chrome reduction into small toxicity, the trivalent chromium of animal migration difference, its precipitation is set to be fixed up, so that by pollution source area Pollutant abatement is fixed, and prevents it to around spreading, and is conducive to reaching the target that further control is eliminated.But nano iron particles It is small, so easily reunite, oxidizable inactivation, therefore, solve the agglomeration traits of Nanoscale Iron and improve stability, the heat as research Point.
Li Chenhua exists《Cr VI research in alta-mud loaded nano iron removal underground water》In, using FeSO4·7H2O and sodium Base bentonite is prepared for a kind of adsorbent of removal Cr VI, but also there is small specific surface area, Nanoscale Iron easy in inactivation, absorption The low problem of efficiency.
The content of the invention
Think deeply based on more than, the present invention is intended to provide a kind of specific surface area is big, adsorption efficiency is high, long service life swelling Earth adsorbing.
The technical problems to be solved by the invention are realized using following technical scheme：
A kind of load Nanoscale Iron bentone adsorbent sterilized for metallurgical briquetting zinc ion, it is characterised in that be by following heavy The raw material for measuring part is made：
Attapulgite 3-5, sodium bentonite 30-50, activated carbon 5-10, hydrochloric acid solution 3-6, silver nitrate solution 10-15, FeSO4·7H2O 10-20, solution of zinc sulfate 3-7, KBH4 5-10, NaOH 20-30, deoxidation appropriate amount of water, deionized water 30-80, Deoxygenated ethanol 20-100, ethanol 20-40；
The mass fraction of the silver nitrate solution is 1-2%；The mass fraction of NaOH solution is 0.1-1%, hydrochloric acid solution quality point Number is 10-15%, and solution of zinc sulfate mass fraction is 30-40%.
The preparation method of described load Nanoscale Iron bentone adsorbent a kind of sterilized for metallurgical briquetting zinc ion, its It is characterised by, is made up of following steps：
A. attapulgite is toasted into 1-3h at 120-160 DEG C, after removing organic compound therein, is scattered in distilled water, Add hydrochloric acid solution, solution of zinc sulfate to be activated and ion exchange absorption, obtain the attapulgite rich in zinc ion, filtering Dry for standby；
B. activated carbon is added in ethanol, after ultrasonic disperse is uniform, soaks 1-2h, filtered and dry；Silver nitrate solution is dripped It is added in the activated carbon of drying, and is stirred continuously, make its wetting uniform, 300- is placed in after then the activated carbon of moistening is dried 20-80min is calcined at 500 DEG C, active carbon loading silver is obtained；
Be added in deionized water for step a gained attapulgite, step b gained active carbon loading silver, sodium bentonite by c, continues Stirring 20-25h, after making its fully dispersed, is added thereto to FeSO4·7H2O, then persistently after stirring 20-25h, in nitrogen protection Under, add deoxygenated ethanol；
D. by KBH4It is dissolved in NaOH, is added drop-wise under stirring condition in step c gained suspensions, occurs black precipitate immediately；Drop Add after finishing, persistently stir 20-40min, filter and washed 2-3 times with deoxygenated water, deoxygenated ethanol, dry, obtain final product load nanometer Iron, silver, the bentone adsorbent of activated carbon.
The preparation method of described load Nanoscale Iron bentone adsorbent a kind of sterilized for metallurgical briquetting zinc ion, its It is characterised by, sodium bentonite used was using preceding needing 200-300 mesh sieves.
The beneficial effects of the invention are as follows：KBH4Ferrous iron can be reduced to Zero-valent Iron in the basic conditions, stick to swelling On soil, the shortcoming of Nanoscale Iron bad dispersibility limitation application is solved, the extensive use of economical clay mineral is conducive to again；Nanometer Iron effectively by hexavalent chrome reduction into small toxicity, the trivalent chromium of animal migration difference can make its precipitation be fixed up, so that will pollution The pollutant abatement of source region is fixed, and prevents it to around spreading, and is conducive to reaching the target that further control is eliminated；Silver nitrate leads to Crossing high-temperature calcination can generate elemental silver, and load on the activated carbon, is introduced into absorption system, and one side activated carbon can increase swollen Moisten the specific surface area of soil, so as to increase the contact area of adsorbent and pollutant, improve adsorption efficiency；Another aspect silver particles can To activate the nanometer iron catalyst for having inactivated, catalysis activity, clean-up effect are improved, while increasing the service life；Coordinate addition Zinc ion there is sterilized and anti-detonation.
Specific embodiment
Specific embodiment of the invention is further described with reference to embodiment.
Embodiment
A kind of load Nanoscale Iron bentone adsorbent sterilized for metallurgical briquetting zinc ion, it is characterised in that be by with The raw material of lower weight portion is made：
Attapulgite 5, sodium bentonite 50, activated carbon 10, hydrochloric acid solution 6, silver nitrate solution 15, FeSO4·7H2O 20, sulphur Sour zinc solution 7, KBH4 10, NaOH 30, deoxidation appropriate amount of water, deionized water 80, deoxygenated ethanol 100, ethanol 40；
The mass fraction of the silver nitrate solution is 1-2%；The mass fraction of NaOH solution is 0.1-1%, hydrochloric acid solution quality point Number is 10-15%, and solution of zinc sulfate mass fraction is 30-40%.
The preparation method of described load Nanoscale Iron bentone adsorbent a kind of sterilized for metallurgical briquetting zinc ion, its It is characterised by, is made up of following steps：
A. attapulgite is toasted into 1-3h at 120-160 DEG C, after removing organic compound therein, is scattered in distilled water, Add hydrochloric acid solution, solution of zinc sulfate to be activated and ion exchange absorption, obtain the attapulgite rich in zinc ion, filtering Dry for standby；
B. activated carbon is added in ethanol, after ultrasonic disperse is uniform, soaks 1-2h, filtered and dry；Silver nitrate solution is dripped It is added in the activated carbon of drying, and is stirred continuously, make its wetting uniform, 300- is placed in after then the activated carbon of moistening is dried 20-80min is calcined at 500 DEG C, active carbon loading silver is obtained；
Be added in deionized water for step a gained attapulgite, step b gained active carbon loading silver, sodium bentonite by c, continues Stirring 20-25h, after making its fully dispersed, is added thereto to FeSO4·7H2O, then persistently after stirring 20-25h, in nitrogen protection Under, add deoxygenated ethanol；
D. by KBH4It is dissolved in NaOH, is added drop-wise under stirring condition in step c gained suspensions, occurs black precipitate immediately；Drop Add after finishing, persistently stir 20-40min, filter and washed 2-3 times with deoxygenated water, deoxygenated ethanol, dry, obtain final product load nanometer Iron, silver, the bentone adsorbent of activated carbon.
The preparation method of described load Nanoscale Iron bentone adsorbent a kind of sterilized for metallurgical briquetting zinc ion, its It is characterised by, sodium bentonite used was using preceding needing 200-300 mesh sieves.
Performance test data of the invention is：After reaction 40min, hexavalent chromium removal rate >=90%.

Claims (3)

1. a kind of load Nanoscale Iron bentone adsorbent sterilized for metallurgical briquetting zinc ion, it is characterised in that be by following The raw material of weight portion is made：
Attapulgite 3-5, sodium bentonite 30-50, activated carbon 5-10, hydrochloric acid solution 3-6, silver nitrate solution 10-15, FeSO4· 7H2O 10-20, solution of zinc sulfate 3-7, KBH4 5-10, NaOH 20-30, deoxidation appropriate amount of water, deionized water 30-80, deoxidation second Alcohol 20-100, ethanol 20-40；
The mass fraction of the silver nitrate solution is 1-2%；The mass fraction of NaOH solution is 0.1-1%, hydrochloric acid solution quality point Number is 10-15%, and solution of zinc sulfate mass fraction is 30-40%.
2. a kind of load Nanoscale Iron bentone adsorbent sterilized for metallurgical briquetting zinc ion according to claim 1 Preparation method, it is characterised in that be made up of following steps：
A. attapulgite is toasted into 1-3h at 120-160 DEG C, after removing organic compound therein, is scattered in distilled water, Add hydrochloric acid solution, solution of zinc sulfate to be activated and ion exchange absorption, obtain the attapulgite rich in zinc ion, filtering Dry for standby；
B. activated carbon is added in ethanol, after ultrasonic disperse is uniform, soaks 1-2h, filtered and dry；Silver nitrate solution is dripped It is added in the activated carbon of drying, and is stirred continuously, make its wetting uniform, 300- is placed in after then the activated carbon of moistening is dried 20-80min is calcined at 500 DEG C, active carbon loading silver is obtained；
Be added in deionized water for step a gained attapulgite, step b gained active carbon loading silver, sodium bentonite by c, continues Stirring 20-25h, after making its fully dispersed, is added thereto to FeSO4·7H2O, then persistently after stirring 20-25h, in nitrogen protection Under, add deoxygenated ethanol；
D. by KBH4It is dissolved in NaOH, is added drop-wise under stirring condition in step c gained suspensions, occurs black precipitate immediately；Drop Add after finishing, persistently stir 20-40min, filter and washed 2-3 times with deoxygenated water, deoxygenated ethanol, dry, obtain final product load nanometer Iron, silver, the bentone adsorbent of activated carbon.
3. a kind of load Nanoscale Iron bentone adsorbent sterilized for metallurgical briquetting zinc ion according to claim 2 Preparation method, it is characterised in that sodium bentonite used was using preceding needing 200-300 mesh sieves.
CN201611198510.XA 2016-12-22 2016-12-22 A kind of load Nanoscale Iron bentone adsorbent sterilized for metallurgical briquetting zinc ion and preparation method thereof Pending CN106807327A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019042906A1 (en) * 2017-08-29 2019-03-07 Merck Patent Gmbh Laser additive and additive for lds plastics
CN114713837A (en) * 2022-04-20 2022-07-08 桂林电子科技大学 Nano zero-valent iron-carbon ceramsite, preparation method thereof and application thereof in wastewater treatment

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CN103496711A (en) * 2013-09-10 2014-01-08 叶香雄 Preparation method of antibacterial attapulgite
CN104785202A (en) * 2015-04-21 2015-07-22 南京林业大学 Preparation method for modified attapulgite adsorbing agent
CN105817209A (en) * 2016-05-20 2016-08-03 张能力 Active carbon water treatment composite adsorbent and preparing method thereof
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CN103496711A (en) * 2013-09-10 2014-01-08 叶香雄 Preparation method of antibacterial attapulgite
CN103464091A (en) * 2013-10-08 2013-12-25 武汉科技大学 Modified bentonite load nanometer iron material and preparation method thereof
CN104785202A (en) * 2015-04-21 2015-07-22 南京林业大学 Preparation method for modified attapulgite adsorbing agent
CN105854797A (en) * 2016-04-11 2016-08-17 中国矿业大学 Preparation method and application of nanometer zero-valence bimetal-supported functional charcoal
CN105817209A (en) * 2016-05-20 2016-08-03 张能力 Active carbon water treatment composite adsorbent and preparing method thereof

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019042906A1 (en) * 2017-08-29 2019-03-07 Merck Patent Gmbh Laser additive and additive for lds plastics
CN114713837A (en) * 2022-04-20 2022-07-08 桂林电子科技大学 Nano zero-valent iron-carbon ceramsite, preparation method thereof and application thereof in wastewater treatment

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