CN105944664A - Preparation method of magnetically separable NiFe2O4/ SBA-15 composite material - Google Patents
Preparation method of magnetically separable NiFe2O4/ SBA-15 composite material Download PDFInfo
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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
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
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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
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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
- B01J20/28002—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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
- B01J20/3204—Inorganic carriers, supports or substrates
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
- B01J20/3234—Inorganic material layers
- B01J20/3236—Inorganic material layers containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a preparation method of a magnetically separable NiFe2O4/SBA-15 composite material. The material is an excellent magnetic adsorbent prepared by filling an ordered mesopore SBA-15 porous channel with a certain amount of magnetic NiFe2O4 nano-particles. The preparation method comprises the steps of 1, weighing right amount of SBA-15 and metal salt according to certain mole ratio; 2, adding the weighed materials into right amount of anhydrous ethanol, stirring at the constant temperature until completely dry, then adding right amount of n-hexane, and stirring until dry to obtain powder; 3, calcining the obtained powder to obtain the NiFe2O4/ SBA-15 composite material. The composite material prepared by the preparation method can be used for absorbing organic dyestuff in sewage, and has the advantages that 1, the SBA-15 has a larger specific surface area, and generates more small holes after being filled with the NiFe2O4, thus having good adsorption capacity; 2, the composite material contains the magnetic NiFe2O4, thus having good magnetic response and being easily recycled from the sewage by means of magnetic separation; 3, the composite material is simple to prepare and easy to operate.
Description
Technical field
The present invention relates to one can Magneto separate NiFe2O4The preparation method of/SBA-15 composite, by a small amount of NiFe2O4It is filled in SBA-15 duct.
Background technology
China is DYE PRODUCTION big country, and dye industry is the most fast-developing, and according to statistics, within 2015, China's various dyestuff yield has reached about 1,150,000 tons.These organic dyestuff are widely used in such as textile, leather, cosmetics, papermaking, printing, plastics etc. industry, thus create substantial amounts of waste water from dyestuff, and environment and the mankind can be brought huge harm by the organic dyestuff in these sewage.Additionally, along with people are more and more higher to the needs of color, the kind of dyestuff also gets more and more, and becomes increasingly difficult to photodissociation, oxidation, biodegradation, this makes these waste water become increasingly difficult to process.Physical absorption by as a kind of simple effectively and the method for environmental protection and economy is used to remove the dyestuff in waste water, and adsorbent used can also by some in more economical way material obtained by simple method.The specific surface area of SBA-15 can be more than 700 m2·g-1, it is the adsorbent of a kind of great potential.
Filtration is the method that traditional adsorbent separates and recovers from sewage, but the method usually can cause filter net jam and break down and cause again polluting, and is not a kind of effective recovering means.At present, magnetic separation technique as one simply, recovering means fast and effectively, obtained people and paid close attention to widely.If by SBA-15 with magnetisable material (such as NiFe2O4) be combined with each other and make magnetic adsorbent, not only can solve the purifying problem of organic dyestuff in sewage, solve simultaneously adsorbent complete absorption after efficiently separate recovery problem.
Summary of the invention
The present invention be in order to prepare a kind of in sewage can Magneto separate, easily prepared organic dye adsorbent namely, and provide one can Magneto separate NiFe2O4The preparation method of/SBA-15 composite.
SBA-15, as a kind of mesopore molecular sieve, has the various features such as pore size distribution is uniform, aperture is adjustable, specific surface area is big, hydrothermal stability is high, has a good application prospect at adsorbent neighborhood.
NiFe2O4Deng as a kind of soft magnetic materials, there is the magnetic property of excellence, the method for Magneto separate can be used effectively and rapidly to separate from sewage.
The present invention has synthesized SBA-15 nano composite material by simple infusion process, loads a small amount of NiFe in the duct of SBA-152O4, by the effect of external magnetic field, adsorbent can be separated from sewage, SBA-15 and load NiFe2O4Mass ratio can adjust according to practical situation.
One can Magneto separate NiFe2O4The preparation method of/SBA-15 composite, is specifically realized by the following steps: one, by silicon (being provided by SBA-15), ferrum (by Fe (NO3)3·9H2O provide) and nickel (by Ni (NO3)2·6H2O provides) atomic ratio is that 1:0.1:0.05 ~ 1:0.5:0.25 weighs appropriate SBA-15, Fe (NO3)3·9H2O and Ni (NO3)2·6H2O；Two, above-mentioned material is joined jointly in politef cup, and add 20 mL dehydrated alcohol, again politef cup is put in water bath with thermostatic control cup, stir the mixture for being completely dried under 45 DEG C of constant temperature, be subsequently adding 20 mL normal hexane and stir to being completely dried and obtain powder；Three, gained powder put in Muffle furnace 700 DEG C of calcinings 6 hours are the most available can Magneto separate NiFe2O4/ SBA-15 composite.
The invention have the advantages that one, SBA-15 has bigger specific surface area, and at NiFe2O4Producing more aperture after filling, absorbability is splendid；Two, composite is containing being magnetic NiFe2O4, there is good magnetic response, easily Magneto separate recycling from sewage；Three, composite preparation is simple, easily operates.
Accompanying drawing explanation
Being prepared for according to detailed description of the invention three can Magneto separate NiFe2O4/ SBA-15 composite, wherein Fig. 1 is the NiFe of experiment synthesis2O4The XRD figure spectrum of/SBA-15；Fig. 2 is the NiFe of synthesis2O4The VSM curve of/SBA-15；Fig. 3 is NiFe2O4/ SBA-15 external magnetic field response condition photo, is by NiFe in picture2O4/ SBA-15 places the response condition observing its external magnetic field in water, and wherein external magnetic field Surface field size is 1800 Oe.
Detailed description of the invention
Detailed description of the invention one: one, by silicon (being provided by SBA-15), ferrum (by Fe (NO3)3·9H2O provide) and nickel (by Ni (NO3)2·6H2O provides) atomic ratio is that 1:0.1:0.05 weighs appropriate SBA-15(1.00 gram), Fe (NO3)3·9H2O(about 0.67 gram) and Ni (NO3)2·6H2O(about 0.24 gram)；Two, above-mentioned material is joined jointly in politef cup, and add 20 mL dehydrated alcohol, again politef cup is put in water bath with thermostatic control cup, stir the mixture for being completely dried under 45 DEG C of constant temperature, be subsequently adding 20 mL normal hexane and stir to being completely dried and obtain powder；Three, gained powder put in Muffle furnace 700 DEG C of calcinings 6 hours are the most available can Magneto separate NiFe2O4/ SBA-15 composite.
Detailed description of the invention two: one, by silicon (being provided by SBA-15), ferrum (by Fe (NO3)3·9H2O provide) and nickel (by Ni (NO3)2·6H2O provides) atomic ratio is that 1:0.2:0.1 weighs appropriate SBA-15(1.00 gram), Fe (NO3)3·9H2O(about 1.34 grams) and Ni (NO3)2·6H2O(about 0.48 gram)；Two, above-mentioned material is joined jointly in politef cup, and add 20 mL dehydrated alcohol, again politef cup is put in water bath with thermostatic control cup, stir the mixture for being completely dried under 45 DEG C of constant temperature, be subsequently adding 20 mL normal hexane and stir to being completely dried and obtain powder；Three, gained powder put in Muffle furnace 500 DEG C of calcinings 6 hours are the most available can Magneto separate NiFe2O4/ SBA-15 composite.
Detailed description of the invention three: one, by silicon (being provided by SBA-15), ferrum (by Fe (NO3)3·9H2O provide) and nickel (by Ni (NO3)2·6H2O provides) atomic ratio is that 1:0.3:0.15 weighs appropriate SBA-15(1.00 gram), Fe (NO3)3·9H2O(about 2.02 grams) and Ni (NO3)2·6H2O(about 0.73 gram)；Two, above-mentioned material is joined jointly in politef cup, and add 20 mL dehydrated alcohol, again politef cup is put in water bath with thermostatic control cup, stir the mixture for being completely dried under 45 DEG C of constant temperature, be subsequently adding 20 mL normal hexane and stir to being completely dried and obtain powder；Three, gained powder put in Muffle furnace 600 DEG C of calcinings 7 hours are the most available can Magneto separate NiFe2O4/ SBA-15 composite.
Detailed description of the invention four: one, by silicon (being provided by SBA-15), ferrum (by Fe (NO3)3·9H2O provide) and nickel (by Ni (NO3)2·6H2O provides) atomic ratio is that 1:0.4:0.2 weighs appropriate SBA-15(1.00 gram), Fe (NO3)3·9H2O(about 2.69 grams) and Ni (NO3)2·6H2O(about 0.97 gram)；Two, above-mentioned material is joined jointly in politef cup, and add 20 mL dehydrated alcohol, again politef cup is put in water bath with thermostatic control cup, stir the mixture for being completely dried under 45 DEG C of constant temperature, be subsequently adding 20 mL normal hexane and stir to being completely dried and obtain powder；Three, gained powder put in Muffle furnace 700 DEG C of calcinings 6 hours are the most available can Magneto separate NiFe2O4/ SBA-15 composite.
Detailed description of the invention five: one, by silicon (being provided by SBA-15), ferrum (by Fe (NO3)3·9H2O provide) and nickel (by Ni (NO3)2·6H2O provides) atomic ratio is that 1:0.5:0.25 weighs appropriate SBA-15(1.00 gram), Fe (NO3)3·9H2O(about 3.36 grams) and Ni (NO3)2·6H2O(about 1.21 grams)；Two, above-mentioned material is joined jointly in politef cup, and add 20 mL dehydrated alcohol, again politef cup is put in water bath with thermostatic control cup, stir the mixture for being completely dried under 45 DEG C of constant temperature, be subsequently adding 20 mL normal hexane and stir to being completely dried and obtain powder；Three, gained powder put in Muffle furnace 700 DEG C of calcinings 8 hours are the most available can Magneto separate NiFe2O4/ SBA-15 composite.
Above-mentioned detailed description of the invention is exemplary, it is to preferably make to skilled artisans appreciate that the present invention, it is not to be construed as the present invention is included the restriction of scope, as long as any equivalent change made according to disclosed spirit or modification, each fall within the scope that the present invention includes.
Claims (2)
1. one kind can Magneto separate NiFe2O4The preparation method of/SBA-15 composite, it is characterised in that be use simple infusion process synthesis, specifically comprise the following steps that one, by silicon (being provided by SBA-15), ferrum (by Fe (NO3)3·9H2O provide) and nickel (by Ni (NO3)2·6H2O provides) atomic ratio is that 1:0.1:0.05 ~ 1:0.5:0.25 weighs appropriate SBA-15, Fe (NO3)3·9H2O and Ni (NO3)2·6H2O；Two, above-mentioned material is joined jointly in politef cup, and add 20 mL dehydrated alcohol, again politef cup is put in water bath with thermostatic control cup, stir the mixture for being completely dried under 45 DEG C of constant temperature, be subsequently adding 20 mL normal hexane and stir to being completely dried and obtain powder；Three, gained powder put in Muffle furnace 500 ~ 700 DEG C of calcinings 6 ~ 8 hours are the most available can Magneto separate NiFe2O4/ SBA-15 composite.
One the most according to claim 1 can Magneto separate NiFe2O4The preparation method of/SBA-15 composite, it is characterised in that be filled with a small amount of NiFe with magnetic response characteristic in the duct of order mesoporous SBA-152O4Nanoparticle.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107132252A (en) * | 2017-05-23 | 2017-09-05 | 徐靖才 | A kind of preparation method of tin dope nickel oxide gas sensitive |
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Application publication date: 20160921 |