CN105413630A - Magnetic medical stone composite adsorption material and preparing method thereof - Google Patents

Magnetic medical stone composite adsorption material and preparing method thereof Download PDF

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Publication number
CN105413630A
CN105413630A CN201610040232.9A CN201610040232A CN105413630A CN 105413630 A CN105413630 A CN 105413630A CN 201610040232 A CN201610040232 A CN 201610040232A CN 105413630 A CN105413630 A CN 105413630A
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medical stone
magnetic
stone composite
magnetic medical
preparing method
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陈世界
乔成立
李英杰
吕仁江
高立娣
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Qiqihar University
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Qiqihar University
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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
    • B01J20/165—Natural alumino-silicates, e.g. zeolites
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Water Treatment By Sorption (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a magnetic medical stone composite adsorption material and a preparing method thereof. The preparing method comprises specific steps: (1) calcinating natural medical stone for 3-5h at 400-500 DEG C, then passing by a 60-mesh sieve for standby; (2) taking a proper amount of FeCl3.6H2O, dissolving in certain amount of ethylene glycol, and performing magnetic stirring for 0.5h to obtain a yellow transparent solution; (3) adding a proper amount of anhydrous NaAc into the obtained solution in step (2), then adding certain amount of the medical stone treated in step (1) and transferring the obtained solution into a 50mL reaction kettle with a polytetrafluoroethylene liner; (4) placing in an oven, placing for 8-12h at 200 DEG C, and taking out of the reaction kettle after reaction and cooling to room temperature; (5) washing an obtained material with deionized water for three times, then washing with ethyl alcohol for three times, and performing vacuum drying for 12h at 60 DEG C, thus obtaining the magnetic medical stone composite adsorption material. The prepared Fe3O4/magnetic medical stone is high in purity, stable in performance, difficult to deteriorate in air and good in adsorption performance.

Description

A kind of magnetic medical stone composite adsorbing material and preparation method thereof
Technical field
The present invention relates to a kind of magnetic medical stone composite adsorbing material and preparation method thereof, belong to the preparing technical field of inorganic nano material.
Background technology
Medical stone has certain bioactive medicinal rock or complex mineral.Its chemical composition is inorganic silicon-aluminum hydrochlorate mainly.Comprising FeO, Al 2o 3, SiO 2, Fe 2o 3, CaO, MgO, K 2o, TiO 2, Na 2o, MnO, P 2o 5deng, also comprise the required all macroelements of animal, such as: the trace element such as Na, Ca, K, Mg, Mo, Cu and rare earth element etc., about 58 kinds.
Medical stone essential mineral has anorthite, quartz, potassium albite, plagioclase etc., and the clay-type substance that its inside is rich in is kaolin, flakey biotite, hydromica, carbonate etc., and protolith mostly is quartz porphyry, quartz diorite, granodiorite etc.The medical stone occurrence of various places institute output, rock form and chemical composition is substantially identical.Absorption affinity is strong, and so-called absorption is the solvation having the solid of porous and huge surface area whole, and then the reaction of chemistry and physics can occur.Medical stone as during Chinese medicine to skin disease, especially draw out the pus, effect is very good.Because medical stone has porous, research shows, medical stone can adsorb harmful components, also can well adsorb organic matter.Absorption affinity is strong especially, from its main component be silica, this point of aluminium oxide considers, be readily appreciated that.Observing medical stone attritive powder in electron micrograph, confirmed that it is spongy porous, is that it has the maximum reason of adsorptivity.That is, because have porous, so its surface area is very large.
In recent years, because medical stone has unique structure of matter, some trace elements very useful to human body of energy stripping, therefore it has very large advantage in Drinking Water.If often drink through medical stone treated water, so can well supplement mineral, trace element that needed by human body is wanted, and medical stone mineral water can accelerate blood circulation, and can get rid of toxin residual in human body, be very useful to the body of people.
Publication number be CN1131098C patent document discloses a kind of compound Chinese medicinal stone and preparation method thereof, compound Chinese medicinal stone is by the sintered body load TiO of the mixture of natural medical stone powder and reduced iron powder 2the photosensitive catalyst film composition in surface of+Ag or copper or platinum or palladium nano-particles.In its sintered body, medical stone and reduced iron powder weight ratio are 100: 5 ~ 40, the TiO of light-sensitive catalyst film 2be 100: 0.5 ~ 3 with the weight ratio of Ag or copper or platinum or palladium.The preparation of this compound Chinese medicinal stone is first by medical stone powder and reduced iron powder mixing; adding additives kneading is agglomerating again; by usual sintering process at 1100 ~ 1350 DEG C of sintering, cool to obtain particle or post or pie sintered body, then be carrier with sintered body, at deposited on supports or lining one deck TiO 2+ light-sensitive catalyst film and making.This compound Chinese medicinal stone can use with various solid form.For purification of water quality and health care aspect, can reclaim, reuse, can reduce use cost, the heavy metal ion of energy catalytic degradation absorption, organic molecule, viral germ, can exempt secondary pollution.
Publication number is the water that patent document discloses a kind of medical stone synthesis ball and preparation method thereof and purified by it of CN102949982B, that 40 ~ 80 object medical stone granule :s are repeatedly calcined in boiler, when temperature reaches 500 DEG C, 1000 DEG C, 1500 DEG C, 2000 DEG C, 2500 DEG C, 3000 DEG C respectively, each maintenance calcining in 1 ~ 2 hour, respectively after cooling, with the speed of 1L/s, extract 0.5 ~ 1 hour, pump impurity, obtain the medical stone granule: of purifying, then after compressing, polishing obtained high-purity medical stone synthesis ball.Soak described medical stone synthesis ball bubble in water 0.5 ~ 2 hour, take out medical stone synthesis ball, can purified water be purified.Due to by medical stone granule: through calcining repeatedly with pump impurity, purity improves greatly, and adsorption capacity strengthens, and has stronger absorption and metathesis to poisonous and harmful substances such as the heavy metal ion in water, organic matter, germs, makes the cleaner health of water sweet.
There is bad dispersibility in the medical stone composite material adsorbent provided in above-mentioned document, recovery difficulty even causes the shortcomings such as secondary pollution mostly.Therefore, exploitation had both had good adsorption effect, and the adsorbent that can conveniently reclaim again has broad prospects.
In recent years, magnetic adsorptive material reclaims the existing relevant report such as heavy metal and organic wastewater in absorption, but the fluoroquinolone antibiotics such as Norfloxacin, Ciprofloxacin report is very few in adsorption treatment water.Therefore, the present invention Fe that utilized solvent-thermal method to prepare 3o 4/ medical stone magnetic coupling sorbing material, for the research and development of expanding emerging micropollutants in magnetic adsorptive material Adsorption water provides Technical Reference.
Summary of the invention
The object of the present invention is to provide a kind of magnetic medical stone composite adsorbing material and preparation method thereof, prepare the undesirable difficult problem of medical stone material recovery to be directed to, provide the preparation method that a kind of technique simply has ordered magnetism medical stone.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of magnetic medical stone composite adsorbing material, and concrete steps are as follows:
(1) natural medical stone is at 400 ~ 500 DEG C of calcining 3 ~ 5h, after 60 mesh sieve, for subsequent use;
(2) appropriate FeCl is got 36H 2o is dissolved in a certain amount of ethylene glycol, and magnetic agitation 0.5h, obtains yellow transparent solution;
(3) add appropriate anhydrous Na Ac in the solution then obtained in step (2), then add a certain amount of maifanite powder after step (1) process, gained solution proceeds in the band teflon-lined reactor of 50mL;
(4) be put in baking oven, 200 DEG C, place 8 ~ 12h, reacted rear taking-up reactor and be cooled to room temperature;
(5) obtain material deionized water and wash three times, then wash three times with ethanol, then through 60 DEG C of vacuum drying 12h, both obtain magnetic medical stone composite adsorbing material.
The invention has the beneficial effects as follows: the magnetic medical stone obtained with the present invention is micro-nano structure, obtained Fe 3o 4/ medical stone magnetic medical stone purity is high, stable performance, and mutability, absorption property are not good in atmosphere.Present invention process is simple, and low for equipment requirements, raw material are easy to get, low cost, can produce in enormous quantities, is convenient to reclaim.Fe prepared by the present invention 3o 4/ medical stone magnetic coupling sorbing material and preparation method thereof is conducive to the unique performance and application of modification medical stone fluoroquinolone antibiotics such as Norfloxacin, Ciprofloxacin in water itself and effectively removes.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further described.
Fig. 1 is the preparation flow figure of magnetic medical stone composite adsorbing material of the present invention.
Fig. 2 is the stereoscan photograph of the magnetic medical stone composite adsorbing material of embodiment 1.
Fig. 3 is the transmission electron microscope photo of the magnetic medical stone composite adsorbing material of embodiment 1.
Fig. 4 is BET adsorption-desorption isothermal and the pore size distribution curve of the magnetic medical stone composite adsorbing material of embodiment 1.
Fig. 5 is the adsorption experiment magnetic display schematic diagram of the magnetic medical stone composite adsorbing material adopting this method to prepare.
Detailed description of the invention
Embodiment 1
A preparation method for magnetic medical stone composite adsorbing material, concrete steps are as follows:
(1) natural medical stone is at 400 DEG C of calcining 4h, after 60 mesh sieve, for subsequent use;
(2) by the FeCl of 2.7g 36H 2o is dissolved in 100mL ethylene glycol, and magnetic agitation 0.5h, obtains yellow transparent solution;
(3) add 7.2g anhydrous Na Ac in the solution then obtained in step (2), then add the 1.0g maifanite powder after step (1) process, gained solution proceeds in the band teflon-lined reactor of 50mL;
(4) be put in baking oven, 200 ° of C, place 8h.React rear taking-up reactor and be cooled to room temperature;
(5) resulting materials deionized water washes three times, then washes three times with ethanol, then through 60 DEG C of vacuum drying 12h, both obtains Fe 3o 4/ medical stone magnetic coupling sorbing material.
Embodiment 2
A preparation method for magnetic medical stone composite adsorbing material, concrete steps are as follows:
(1) natural medical stone is at 500 DEG C of calcining 5h, after 60 mesh sieve, for subsequent use;
(2) by the FeCl of 2.7g 36H 2o is dissolved in 100mL ethylene glycol, and magnetic agitation 0.5h, obtains yellow transparent solution;
(3) add 7.2g anhydrous Na Ac in the solution then obtained in step (2), then add the 1.0g maifanite powder after step (1) process, gained solution proceeds in the band teflon-lined reactor of 50mL;
(4) be put in baking oven, 200 ° of C, place 10h.React rear taking-up reactor and be cooled to room temperature;
(5) resulting materials deionized water washes three times, then washes three times with ethanol, then through 60 DEG C of vacuum drying 12h, both obtains Fe 3o 4/ medical stone magnetic coupling sorbing material.
Embodiment 3
A preparation method for magnetic medical stone composite adsorbing material, concrete steps are as follows:
(1) natural medical stone is at 400 DEG C of calcining 4h, after 60 mesh sieve, for subsequent use;
(2) by the FeCl of 0.82g 36H 2o is dissolved in 40mL ethylene glycol, and magnetic agitation 0.5h, obtains yellow transparent solution;
(3) add 3.6g anhydrous Na Ac in the solution then obtained in step (2), then add the 0.4g maifanite powder after step (1) process, gained solution proceeds in the band teflon-lined reactor of 50mL;
(4) be put in baking oven, 200 ° of C, place 12h.React rear taking-up reactor and be cooled to room temperature;
(5) resulting materials deionized water washes three times, then washes three times with ethanol, then through 60 DEG C of vacuum drying 12h, both obtains Fe 3o 4/ medical stone magnetic coupling sorbing material.

Claims (1)

1. a preparation method for magnetic medical stone composite adsorbing material, is characterized in that: concrete steps are as follows:
(1) natural medical stone is at 400 ~ 500 DEG C of calcining 3 ~ 5h, after 60 mesh sieve, for subsequent use;
(2) appropriate FeCl is got 36H 2o is dissolved in a certain amount of ethylene glycol, and magnetic agitation 0.5h, obtains yellow transparent solution;
(3) add appropriate anhydrous Na Ac in the solution then obtained in step (2), then add a certain amount of maifanite powder after step (1) process, gained solution proceeds in the band teflon-lined reactor of 50mL;
(4) be put in baking oven, 200 DEG C, place 8 ~ 12h, reacted rear taking-up reactor and be cooled to room temperature;
(5) obtain material deionized water and wash three times, then wash three times with ethanol, then through 60 DEG C of vacuum drying 12h, both obtain magnetic medical stone composite adsorbing material.
CN201610040232.9A 2016-01-21 2016-01-21 Magnetic medical stone composite adsorption material and preparing method thereof Pending CN105413630A (en)

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Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104826600A (en) * 2015-05-05 2015-08-12 济南大学 Preparation method of magnetic kaolin
CN104826602A (en) * 2015-05-05 2015-08-12 济南大学 Preparation method of magnetism-loaded medical stone powder material
CN104826601A (en) * 2015-05-05 2015-08-12 济南大学 Preparation method of magnetic diatomite

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104826600A (en) * 2015-05-05 2015-08-12 济南大学 Preparation method of magnetic kaolin
CN104826602A (en) * 2015-05-05 2015-08-12 济南大学 Preparation method of magnetism-loaded medical stone powder material
CN104826601A (en) * 2015-05-05 2015-08-12 济南大学 Preparation method of magnetic diatomite

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