CN103495379A - Method for preparing zeolite supported iron oxide - Google Patents

Abstract

The invention discloses a method for preparing zeolite supported iron oxide. The method comprises the following steps: crushing, grinding and sieving natural zeolite to obtain zeolite with particle diameter of 20-40 meshes for later use; (2) soaking the zeolite sieved in the step (1) in hydrochloric acid with mass percentage concentration of 5% for 8-24 h, cleaning the zeolite through ultra pure water until the pH value is neutral, and steaming the zeolite at a temperature of 80-200 DEG C; (3) weighing 100g of Fe (NO3)3 and dissolving the Fe (NO3)3 into 150 ml of ultra pure water; (4) uniformly mixing 400 g of zeolite obtained in the step (2) with the solution obtained in the step (3), stirring for 5-15 min, and drying the mixture in a drying oven for 8-24 h at a temperature of 80-200 DEG C; and (5) cleaning the zeolite obtained in the step (4) through ultra pure water until the pH value of the washed water is neutral, and then, drying the zeolite at a temperature of 80-200 DEG C, and bottling the zeolite for storage. The method disclosed by the invention is simple to operate, low in cost and environment-friendly, and the prepared product can be extensively applied in production procedures of deep sewage dephosphorization and micro-polluted source water quality purification.

Description

The preparation method of zeolite-loaded iron oxide

Technical field

The present invention relates to a kind of zeolite-loaded iron oxide preparation method of (Iron-Oxide-Coated-Zeolite is called for short IOCZ), utilize especially zeolite for main material, studied the preparation method of zeolite-loaded iron oxide.

Background technology

The mankind have caused a series of serious Environmental and ecological problems to the various phosphorus-containing compounds of discharge in environment without limit, are one of principal elements caused water body generation eutrophication.In water, the removal method of phosphorus mainly contains at present: bioanalysis, chemical precipitation method, artificial swamp method, ion-exchange and absorption method etc.Bioanalysis and chemical precipitation method can produce a large amount of phosphorous excess sludges, have improved processing cost, and the recovery of phosphorus also has certain difficulty.The artificial swamp method is not high to the removal efficiency of phosphorus, and its processing cost of ion-exchange is higher.The absorption method dephosphorization relies on the adsorbent of some porous or Large ratio surface and the absorption affinity between the phosphate anion in sewage to carry out the method for adsorption and dephosphorization, and utilizes the absorption-desorption method, can reach and eliminate the dual purpose that phosphorus pollutes and reclaim phosphor resource.This method is compared with chemical precipitation method, produces hardly mud, and treatment facility is simple, and treatment effect is more stable.Ferriferous oxide, due to its higher surface charge and specific area, is commonly used for water treatment absorbent.Usually it is by the molysite as coagulant, in the solution of neutrality or meta-alkalescence, to be generated to precipitate and form.Although the absorption property of ferriferous oxide is fine, metal ion and organic matter are had to higher affine performance, but, because it is a kind of loose, facile hydrolysis, unbodied agglutinating matter, its water guide performance extreme difference, dewater difficult simultaneously, can increase volume and the disposal cost of mud, therefore, fail to be used widely.Should consider removal effect, the sludge quantity generated again is little, and ways of addressing this issue is that ferriferous oxide is loaded on certain carrier, makes it be easy to Separation of Solid and Liquid, and the adsorbent after the adsorption fouling thing is regenerated adsorbent by certain processing.

For the selection of carrier, applying now maximum carriers is the silicates mineral.As iron oxide coated sand (Iron-Oxide-Coated-Sand is called for short IOCS), as the filter tank modified filter material, in removing water, heavy metal (as metals such as Cu, Pb, Cd), organic matter, fluorine, arsenic, phosphorus etc. have research.But up to now, take zeolite as carrier, prepare zeolite-loaded iron oxide and have no report.

Present stage, people have carried out numerous TiO ₂the modification technology of/zeolite, but with regard to nano-TiO ₂itself, its photocatalysis mainly concentrates on ultraviolet region, and relatively less to the utilization of visible ray, zeolite plays booster action in catalytic process, can not fundamentally solve the visible light catalytic problem.In the research of the absorption method dephosphorization in the past adopted, mostly adopt the powdered form adsorbents, although the increase of specific area can adsorption capacity, the Separation of Solid and Liquid difficult is difficult to realize in practice.Zeolite-loaded iron oxide is as a kind of modified filler, not only retained the function that zeolite filler absorption is held back, and increased the activated adoption position at zeolite surface simultaneously, can Adsorption water in dissolubility pollutant.IOCZ not only under neutrallty condition dephosphorizing rate more than 92%; while is Separation of Solid and Liquid very easily; and can be able to regeneration by certain processing mode; therefore the IOCZ adsorption filter has the higher using value that obtains in advanced treatment of wastewater and the purification of micro-pollution sources water quality; carry out the characteristic of IOCZ absorption water pollutant and mechanism research in a deep going way for the protection water body environment, the water treatment technology that ensures drinking water safety and develop the efficient low-consume sustainable use all has great importance.

Summary of the invention

Purpose of the present invention just is to provide a kind of preparation method of zeolite-loaded iron oxide, adopts the iron salt solutions evaporation, take zeolite as primary raw material, take iron oxide and hydrochloric acid as auxiliary material.

Concrete steps are:

(1) natural zeolite is carried out to fragmentation, grinding, obtaining particle diameter after the processing of sieving is that 20 orders-40 purpose zeolite is standby.

(2) the salt acid soak 8-24 hour that the zeolite after step (1) is sieved is 5% with mass percent concentration, till then by ultra-pure water wash clean to pH value, being neutrality, then the zeolite after soaking steams 4-16 hour at 80-200 ℃ of temperature.

(3) take 100g Fe(NO ₃) ₃be dissolved in 150 milliliters of ultra-pure waters.

(4) 400g step (2) gained zeolite is mixed with step (3) gained solution, stir 5-15 minute, in drying box, by 80-200 ℃ of temperature, dry 8-24 hour, cool to room temperature after taking out.

(5) step (4) gained zeolite is cleaned with ultra-pure water, until then the water pH value washed out dries for neutral at 80-200 ℃ of temperature, bottling is preserved.

The present invention is simple for process, owing to utilizing zeolite for main raw material(s), greatly reduces production costs, and has improved the product property indices; Prepared product can be widely used in sewage deep dephosphorization and micro-pollution sources water quality cleaning procedure.

The specific embodiment

Embodiment:

(1) will from the Guilin resource purchasing to natural zeolite carry out fragmentation, grinding, sieving after processing and obtaining particle diameter is that 20 orders-40 purpose zeolite is standby.

(2) the salt acid soak that the zeolite after step (1) is sieved is 5% with mass percent concentration 24 hours, till then by ultra-pure water wash clean to pH value, being neutrality, then the zeolite after soaking steams 12 hours at 120 ℃ of temperature.

(3) take 100g Fe(NO ₃) ₃be dissolved in 150 milliliters of ultra-pure waters.

(4) 400g step (2) gained zeolite is mixed with step (3) gained solution, stir 10 minutes, dry 24 hours by 120 ℃ of temperature in drying box, cool to room temperature after taking out.

(5) step (4) gained zeolite is cleaned with ultra-pure water, until then the water pH value washed out still dries for neutral at 120 ℃ of temperature, bottling is preserved.

The structure of zeolite-loaded ferric oxide particles, one-tenth are grouped into and adopt German Bruker-axs D8ADVANCE type X-ray diffractometer to be tested, sweep limits 2 θ=10-80 °, 4 °/minute of diffraction speed.The pattern of sample and particle diameter adopt ESEM to observe.The Electronic Speculum test adopts the JSM-5610LV type ESEM of NEC, amplifies 300-20000 and doubly carries out morphology observation.

Claims (1)

1. the preparation method of a zeolite-loaded iron oxide is characterized in that concrete steps are:

(1) natural zeolite is carried out to fragmentation, grinding, obtaining particle diameter after the processing of sieving is that 20 orders-40 purpose zeolite is standby;

(2) the salt acid soak 8-24 hour that the zeolite after step (1) is sieved is 5% with mass percent concentration, till then by ultra-pure water wash clean to pH value, being neutrality, then the zeolite after soaking steams 4-16 hour at 80-200 ℃ of temperature;

(3) take 100g Fe(NO ₃) ₃be dissolved in 150 milliliters of ultra-pure waters;

(4) 400g step (2) gained zeolite is mixed with step (3) gained solution, stir 5-15 minute, in drying box, by 80-200 ℃ of temperature, dry 8-24 hour, cool to room temperature after taking out;

(5) step (4) gained zeolite is cleaned with ultra-pure water, until then the water pH value washed out dries for neutral at 80-200 ℃ of temperature, bottling is preserved.