CN105536690A - A preparing method of a manganese zinc ferrite covered with nanometer particles - Google Patents
A preparing method of a manganese zinc ferrite covered with nanometer particles Download PDFInfo
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- CN105536690A CN105536690A CN201510977097.6A CN201510977097A CN105536690A CN 105536690 A CN105536690 A CN 105536690A CN 201510977097 A CN201510977097 A CN 201510977097A CN 105536690 A CN105536690 A CN 105536690A
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- manganese
- zinc ferrite
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- nano particle
- composite yarn
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- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 title claims abstract description 31
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000002245 particle Substances 0.000 title abstract 2
- 239000002253 acid Substances 0.000 claims abstract description 9
- 230000004048 modification Effects 0.000 claims abstract description 5
- 238000012986 modification Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 20
- 239000002131 composite material Substances 0.000 claims description 17
- 239000002105 nanoparticle Substances 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 17
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 12
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 229910000859 α-Fe Inorganic materials 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000011787 zinc oxide Substances 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 229940068984 polyvinyl alcohol Drugs 0.000 claims description 4
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical class [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 230000001476 alcoholic effect Effects 0.000 claims description 2
- 238000004537 pulping Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000696 magnetic material Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract 2
- 239000012528 membrane Substances 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000002699 waste material Substances 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- 239000002351 wastewater Substances 0.000 description 7
- 238000001816 cooling Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000004043 dyeing Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical class [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000005408 paramagnetism Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- 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
- B01J20/0222—Compounds of Mn, Re
-
- 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
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/32—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of manganese, technetium or rhenium
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Materials Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Artificial Filaments (AREA)
- Compounds Of Iron (AREA)
Abstract
A preparing method of a manganese zinc ferrite covered with nanometer particles is disclosed. The method includes steps of (1) preparing a manganese zinc ferrite, (2) preparing an acid solution of the manganese zinc ferrite, (3) performing surface modification and (4) washing and drying. The method is simple and convenient in operation and easy to implement. Through a reasonable formula design and a preparing process, the manganese zinc ferrite magnetic material is evenly covered with an adsorption membrane with a nanoscale thickness and an organic catalyzing membrane with a nanoscale thickness. The prepared manganese zinc ferrite magnetic material is efficient in waste cleaning functions, easy to separate, good in cleaning effects and wide in market prospect.
Description
Technical field
The present invention relates to MnZn ferrite material field, particularly relate to a kind of preparation method of nano particle covered composite yarn manganese-zinc ferrite.
Background technology
Dyeing waste water discharge capacity is large, water quality is complicated, toxicity is large, and containing a large amount of organic pollutions, become to attach most importance to one of environomental pollution source.The features such as absorption method and photocatalysis have that cost is low, no coupling product generates and easy and simple to handle are the effective ways removing Pollutants in Wastewater.Take active carbon as adsorbent, be that photochemical catalyst carries out desolventing technology to dyeing waste water and catalytic decomposition is decolorizing printing and dyeing waste water effective method the most with titania powder, but be no matter all not easily separated and regeneration of active carbon powder or titania powder, be difficult to promote in actual applications.Manganese-zinc ferrite has paramagnetism, and magnetic stability is good, is conducive to stripping down and reusable edible from magnetic separating device.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of preparation method of nano particle covered composite yarn manganese-zinc ferrite.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: the preparation method providing a kind of nano particle covered composite yarn manganese-zinc ferrite, comprises the steps:
(1) prepare manganese-zinc ferrite: with manganese oxide, iron oxide, zinc oxide and calcium carbonate for raw material, through slurrying, grinding and sintering process, prepare MnZn ferrite material;
(2) prepare the acid solution of manganese-zinc ferrite: pulverized by the MnZn ferrite material ball mill grinding of preparation in step (1), be then scattered in acid solution, after ultrasonic disperse is even, add ammoniacal liquor adjust ph;
(3) surface modification: the alcoholic solution adding ethyl orthosilicate and titanate esters in the mixed solution obtained in step (2), reacts under certain condition, then leaves standstill 6 ~ 12h, is cooled to room temperature;
(4) wash, dry: by the product that obtains in step (3) after filtration, washing, dry, obtain described nano particle covered composite yarn MnZn ferrite material.
In a preferred embodiment of the present invention, in described step (1), described raw material dosage is: iron oxide 52 ~ 55mol%, zinc oxide 20 ~ 22mol%, manganese oxide 7 ~ 15mol%, and all the other are calcium carbonate.
In a preferred embodiment of the present invention, in described step (1), described pulping process is that to add the mass concentration accounting for described raw material gross weight 30 ~ 50% be the poly-vinyl alcohol solution of 5%; Described sintering process is under 0.1 ~ 0.2% oxygen concentration, Isothermal sinter 2 ~ 4h at 1450 DEG C.
In a preferred embodiment of the present invention, in described step (2), described acid solution to be molar concentration be 10 ~ 15% citric acid solution; Described pH value is 4 ~ 6; Described grinding rate is 500 ~ 800r/min, and the average grain diameter after grinding is 10 ~ 50nm.
In a preferred embodiment of the present invention, in described step (3), the mol ratio of described ethyl orthosilicate and titanate esters is 1 ~ 3:1; Described reaction condition is: temperature 60 ~ 80 DEG C, stir speed (S.S.) 30 ~ 50r/min, reaction time 1 ~ 3h.
The invention has the beneficial effects as follows: the preparation method of a kind of nano particle covered composite yarn of the present invention manganese-zinc ferrite, it is easy and simple to handle, easy realization, it is by rational formula Design and preparation technology, the adsorbed film of nanometer grade thickness and catalytic organism film in the coated with uniform of manganese-zinc ferrite magnetic material, it has efficient purified treatment effect to waste water, and is easy to be separated, purified treatment is effective, wide market.
Detailed description of the invention
Below preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
The embodiment of the present invention comprises:
Embodiment 1
A preparation method for nano particle covered composite yarn manganese-zinc ferrite, comprises the steps:
(1) manganese-zinc ferrite is prepared: with the manganese oxide of the zinc oxide of the iron oxide of 52mol%, 20mol%, 15mol% and surplus calcium carbonate for raw material, pre-burning 2h at 500 DEG C, add after cooling the mass concentration accounting for described raw material gross weight 30% be 5% poly-vinyl alcohol solution be mixed with slurry, the speed sand milling dispersion 60min of 100r/min, after filtration, oven dry, with Muffle furnace be that under the oxygen concentration of 0.1%, at 1450 DEG C, Isothermal sinter 4h, obtains manganese-zinc ferrite after cooling in volume parts;
(2) acid solution of manganese-zinc ferrite is prepared: ground to average grain diameter as 10 ~ 50nm with the speed of 500r/min by the MnZn ferrite material ball mill of preparation in step (1), being scattered in molar concentration is again in the citric acid solution of 10%, after ultrasonic disperse 1h is extremely even, adding ammoniacal liquor adjust ph is 4;
(3) surface modification: adding mol ratio in the mixed solution obtained in step (2) is the ethyl orthosilicate of 1:1 and the ethanolic solution of titanate esters, at 60 DEG C, reacts 1h under the stir speed (S.S.) of 30r/min, then leaves standstill 6h, is cooled to room temperature;
(4) wash, dry: by the product that obtains in step (3) after filtration, washing, in vacuum drying chamber with dry more than the 4h of the temperature of 60 ~ 80 DEG C, obtain described nano particle covered composite yarn MnZn ferrite material.
Embodiment 2
A preparation method for nano particle covered composite yarn manganese-zinc ferrite, comprises the steps:
(1) manganese-zinc ferrite is prepared: with the manganese oxide of the zinc oxide of the iron oxide of 55mol%, 22mol%, 7mol% and surplus calcium carbonate for raw material, pre-burning 2h at 500 DEG C, add after cooling the mass concentration accounting for described raw material gross weight 50% be 5% poly-vinyl alcohol solution be mixed with slurry, the speed sand milling dispersion 30min of 300r/min, after filtration, oven dry, with Muffle furnace be that under the oxygen concentration of 0.2%, at 1450 DEG C, Isothermal sinter 2h, obtains manganese-zinc ferrite after cooling in volume parts;
(2) acid solution of manganese-zinc ferrite is prepared: ground to average grain diameter as 10 ~ 50nm with the speed of 800r/min by the MnZn ferrite material ball mill of preparation in step (1), being scattered in molar concentration is again in the citric acid solution of 15%, after ultrasonic disperse 1h is extremely even, adding ammoniacal liquor adjust ph is 6;
(3) surface modification: adding mol ratio in the mixed solution obtained in step (2) is the ethyl orthosilicate of 3:1 and the ethanolic solution of titanate esters, at 80 DEG C, reacts 3h under the stir speed (S.S.) of 50r/min, then leaves standstill 12h, is cooled to room temperature;
(4) wash, dry: by the product that obtains in step (3) after filtration, washing, in vacuum drying chamber with dry more than the 4h of the temperature of 60 ~ 80 DEG C, obtain described nano particle covered composite yarn MnZn ferrite material.
The nano particle covered composite yarn manganese-zinc ferrite that said method obtains, the thickness of titanium dioxide and coated by titanium dioxide film is 5 ~ 25nm, reaches more than 95 to the percent of decolourization of waste water, reaches more than 92% to resolution ratio organic in waste water.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (5)
1. a preparation method for nano particle covered composite yarn manganese-zinc ferrite, is characterized in that, comprises the steps:
(1) prepare manganese-zinc ferrite: with manganese oxide, iron oxide, zinc oxide and calcium carbonate for raw material, through slurrying, grinding and sintering process, prepare MnZn ferrite material;
(2) prepare the acid solution of manganese-zinc ferrite: pulverized by the MnZn ferrite material ball mill grinding of preparation in step (1), be then scattered in acid solution, after ultrasonic disperse is even, add ammoniacal liquor adjust ph;
(3) surface modification: the alcoholic solution adding ethyl orthosilicate and titanate esters in the mixed solution obtained in step (2), reacts under certain condition, then leaves standstill 6 ~ 12h, is cooled to room temperature;
(4) wash, dry: by the product that obtains in step (3) after filtration, washing, dry, obtain described nano particle covered composite yarn MnZn ferrite material.
2. the preparation method of nano particle covered composite yarn manganese-zinc ferrite according to claim 1, it is characterized in that, in described step (1), described raw material dosage is: iron oxide 52 ~ 55mol%, zinc oxide 20 ~ 22mol%, manganese oxide 7 ~ 15mol%, and all the other are calcium carbonate.
3. the preparation method of nano particle covered composite yarn manganese-zinc ferrite according to claim 1, is characterized in that, in described step (1), described pulping process is that to add the mass concentration accounting for described raw material gross weight 30 ~ 50% be the poly-vinyl alcohol solution of 5%; Described sintering process is under 0.1 ~ 0.2% oxygen concentration, Isothermal sinter 2 ~ 4h at 1450 DEG C.
4. the preparation method of nano particle covered composite yarn manganese-zinc ferrite according to claim 1, is characterized in that, in described step (2), described acid solution to be molar concentration be 10 ~ 15% citric acid solution; Described pH value is 4 ~ 6; Described grinding rate is 500 ~ 800r/min, and the average grain diameter after grinding is 10 ~ 50nm.
5. the preparation method of nano particle covered composite yarn manganese-zinc ferrite according to claim 1, is characterized in that, in described step (3), the mol ratio of described ethyl orthosilicate and titanate esters is 1 ~ 3:1; Described reaction condition is: temperature 60 ~ 80 DEG C, stir speed (S.S.) 30 ~ 50r/min, reaction time 1 ~ 3h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106943972A (en) * | 2017-05-18 | 2017-07-14 | 南通万宝实业有限公司 | Preparation method for the shell-nuclear compounded structure nano magnetic material of wastewater treatment |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103143359A (en) * | 2013-03-05 | 2013-06-12 | 南京大学 | A magnetic recyclable hollow TiO2-SiO2-CoFe2O4 nano photocatalytic material and its preparation method |
| CN104529426A (en) * | 2014-12-19 | 2015-04-22 | 江门安磁电子有限公司 | High-Bs low-loss manganese-zinc ferrite material applicable to 120-160 DEG C and manufacturing method thereof |
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| CN103143359A (en) * | 2013-03-05 | 2013-06-12 | 南京大学 | A magnetic recyclable hollow TiO2-SiO2-CoFe2O4 nano photocatalytic material and its preparation method |
| CN104529426A (en) * | 2014-12-19 | 2015-04-22 | 江门安磁电子有限公司 | High-Bs low-loss manganese-zinc ferrite material applicable to 120-160 DEG C and manufacturing method thereof |
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| CN106943972A (en) * | 2017-05-18 | 2017-07-14 | 南通万宝实业有限公司 | Preparation method for the shell-nuclear compounded structure nano magnetic material of wastewater treatment |
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