CN104475026A - Novel preparation and application methods of water treatment film doped with MTN-zeolite-configuration composite material - Google Patents

Novel preparation and application methods of water treatment film doped with MTN-zeolite-configuration composite material Download PDF

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CN104475026A
CN104475026A CN201410652665.0A CN201410652665A CN104475026A CN 104475026 A CN104475026 A CN 104475026A CN 201410652665 A CN201410652665 A CN 201410652665A CN 104475026 A CN104475026 A CN 104475026A
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mil
tio
composite
composite material
water treatment
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常娜
余景健
何冬莹
李一新
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Tianjin Polytechnic 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
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
    • 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
    • B01J20/28054—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 surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
    • 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
    • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
    • 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
    • B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
    • 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
    • C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • 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
    • B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
    • B01J2231/70—Oxidation reactions, e.g. epoxidation, (di)hydroxylation, dehydrogenation and analogues
    • 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
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
    • B01J2523/40—Constitutive chemical elements of heterogeneous catalysts of Group IV (IVA or IVB) of the Periodic Table
    • B01J2523/47—Titanium
    • 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
    • B01J2540/00—Compositional aspects of coordination complexes or ligands in catalyst systems
    • B01J2540/60—Groups characterized by their function

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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)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The invention relates to novel preparation and application methods of a water treatment film doped with a MTN-zeolite-configuration composite material. The preparation method specifically comprises the steps of synthesizing porous MIL-100 particles by a hydrothermal method, then, loading pore passages with nano titanium dioxide by adopting a sol method so as to obtain a novel composite material, preparing sol or a suspension from the composite material, coating or painting the surface of a PVDF (polyvinylidene fluoride) film directly with the sol or suspension, and baking, thereby obtaining the novel water treatment film for sewage treatment. The method is simple in process and easy in operation. Shown by adsorption and degradation experiments, the composite material prepared by the method is regular in structure and large in pore capacity and has a good degradation effect on organics, so that a novel adsorption and degradation method for the organics in sewage is developed. According to the method, the added ratio of TiO2-MIL-100 and a polymer and the preparing ratio of the TiO2-MIL-100 suspension are free from any restriction, and the selection of film materials is free from any restriction, so that improvement can be carried out according to research needs or practical application needs.

Description

The preparations and applicatio new method of the water treatment film of doping MTN zeolite configuration composite
Technical field
The present invention relates to a kind of preparations and applicatio new method of water treatment film of the MTN zeolite configuration composite that adulterates.This water treatment film doping advanced composite material (ACM), i.e. load titanium dioxide (TiO 2) the nanocrystalline MIL-100 porous nano particle with MTN zeolite configuration.After water heat transfer porous MIL-100 particle, sol method is adopted to be carried on by nano titanium oxide in its duct, obtain advanced composite material (ACM), above-mentioned composite is prepared into colloidal sol or suspension, direct film or be coated in pvdf membrane surface, and dry, the new type water process film for sewage disposal can be obtained, and finally developed Adsorption of Organic and degraded new method in a kind of sewage.
Background technology
At present, bioanalysis, oxidizing process and physico-chemical process etc. are mainly contained to the processing method of organic wastewater both at home and abroad.Bioanalysis is current most widely used a kind of method for processing organic wastewater, mainly utilizes the metabolism of microorganism, the organic matter be used in degradation of sewage by the cohesion, absorption, oxidation Decomposition etc. of microorganism.Chemical oxidation techniques is usually used in the pretreatment process of carrying out a biological disposal upon, and is generally with chemical oxidizing agent process organic wastewater, to improve the biodegradability of waste water, or the organic matter in direct oxidation degrading waste water.Physico-chemical process process organic pollution mainly contains absorption method, extraction, various membrane technologies etc.Wherein, Membrane Separation for Water Treatment is being most widely used in recent years.
MIL-100 is the rigid backbone porous adsorbing material with MTN zeolite configuration that a class is formed by self assembly effect by metal ion and organic ligand.The well-regulated pore passage structure of MIL-100 tool, (BET specific surface area is up to 3100m for the specific area of super large 2/ g), the remarkable advantages such as good heat endurance and solvent stability, therefore, have been widely used in sample adsorption field.The present invention adopts this novel porous adsorbing material of MIL-100 as adsorbent, comes for the preparation of enrichment and the organic advanced composite material (ACM) of catalytic degradation.
Be used for since catalytic degradation organic matter makes a breakthrough from semi-conducting material, titanium dioxide because its catalytic activity is high, chemistry and biologically inert is good, to human non-toxic, the particular advantages such as inexpensive, become the most active catalysis material of Recent study.Compared with the titanium dioxide of stock size, nano titanium oxide has higher catalytic activity and selective, can form Strong oxdiative-reduction system, decomposed by substance oxidation that is not oxidizable or that be difficult to degrade, this technology has been widely used in the organic wastewater processing the generation of the industry such as dyestuff, papermaking.But because particle diameter is minimum, nano titanium oxide very easily runs off in oxidizing process, therefore, find the carrier can fixing nano titanium oxide, absorption, oxidation Decomposition are combined, is just more conducive to the extensive use in actual production.
The composite that sewerage disposing film of the present invention adulterates is using the porous material MIL-100 of MTN zeolite configuration as binding matrix, after porous MIL-100 materials synthesis, adopt sol method to have the nano titanium oxide of catalytic degradation activity at its duct internal burden, finally make the composite that can be doped in water treatment film.But above-mentioned composite is dispergated fine solid powder, and it has certain limitation in actual water treatment applications, therefore the present invention is intended to the preparation of above-mentioned composite to become form of film, to expand its application in actual water treatment.
This patent system state natural sciences fund (No.21305102), national Students' Innovation foundation drill program (No.201410058026), Tianjin S & T Developmentin High Institutions fund plan (No.2013512), outer academic scientific and technological works contest (No.2014341) funded projects of Tianjin University of Technology's students in class.
Summary of the invention
For realizing technical scheme provided by the present invention be:
Prepare MIL-100 porous adsorbing material with hydro-thermal method, through washing fully, purification, after activation, adopts mortar to be ground into the comparatively homogeneous MIL-100 powder of granularity.MIL-100 powder after overactivation is joined in the ethanolic solution of butyl titanate, drips hydrolyzate and constantly stir, the composite of synthesis of nano titanium dioxide and MIL-100.By composite wash, purification, after activation, namely obtain have MTN zeolite configuration for enrichment and the organic advanced composite material (ACM) of catalytic degradation.
Show through adsorption experiment, TiO prepared by this method 2-MIL-100 composite structure rule, pore capacities is large, to organic absorption and catalytic degradation functional.
Wherein, the hydrothermal synthesis method of porous adsorbing material MIL-100 is: by iron powder, trimesic acid is dissolved in ultra-pure water, hydrofluoric acid, in the mixed liquor of red fuming nitric acid (RFNA), ultrasonic make it dissolve after, mixed solution is placed in polytetrafluoroethylene (PTFE) reactor, carries out pyroreaction in an oven.After reaction terminates, reactor is cooled, the solid matter in reactor is carried out repeatedly, repeatedly washs, with being placed on dry for standby in baking oven.
TiO 2the synthetic method of-MIL-100 composite: take a certain amount of MIL-100 powder, join butyl titanate, in the mixed liquor of ethanol, and stir.Under magnetic agitation condition, in above-mentioned mixed liquor, slowly drip ethanol, water, the mixed liquor of nitric acid, drip and terminate rear continuation stirring some hours.After reaction terminates, centrifugally can obtain salmon pink thick solid.
TiO 2the activation method of-MIL-100 composite: by the washing of above-mentioned salmon pink thick solid ethanol for several times, and solid is placed in baking oven dries, subsequently high-temperature activation a few hours in an oven.
TiO 2the preparation method of-MIL-100 composite water treatment film: by TiO 2-MIL-100 composite dissolves in polymer sol, and direct film is also dried, or by TiO 2-MIL-100 composite dissolves in organic solvent, is coated on pvdf membrane surface, and dries, and can obtain the new type water process film for sewage disposal.
The using method of composite water treatment film: the film of preparation is arranged on supporter in the form of an array, and be placed in cesspool or sewage draining exit, by the porous adsorbing material in film, fast enriching is carried out to the organic matter in sewage, by the TiO of load 2material realizes organic degraded.Meanwhile, sewage sample can carry out sampling monitoring at any time, measures content of organics wherein.
Detailed description of the invention
For better understanding the present invention, below in conjunction with embodiment the present invention done and describe in detail further, but the scope of protection of present invention being not limited to the scope that embodiment represents.
Embodiment:
Prepare MIL-100 porous adsorbing material with hydro-thermal method, adopt sol method to be carried on by nano titanium oxide in MIL-100 sorbing material, composite is purified, after activation, is prepared into for enrichment and the organic advanced composite material (ACM) of catalytic degradation:
The hydrothermal synthesis method of porous adsorbing material MIL-100 is: by 0.2775 gram of iron powder, 0.6875 gram of trimesic acid is dissolved in 25 milliliters of ultra-pure waters, 200 microlitre hydrofluoric acid, in 190 microlitre red fuming nitric acid (RFNA)s, after within ultrasonic 10 minutes, making it dissolve, mixed solution is placed in 30 milliliters of polytetrafluoroethylene (PTFE) reactors, 150 DEG C are reacted 12 hours.Question response still cools, and ultra-pure water, ethanolic solution washs obtained metallic organic framework sorbing material, 200 DEG C of dry for standby.
TiO 2the synthetic method of-MIL-100 composite: adopt mortar MIL-100 to be ground into the comparatively homogeneous powder of granularity.Take 50mg MIL-100 powder, join 25ml butyl titanate, in the mixed liquor of 10ml ethanol, stirred at ambient temperature 1 hour.Under magnetic agitation condition, with the speed of 1ml/min, in above-mentioned mixed liquor, drip 10ml ethanol, 4ml water, the mixed liquor of 1ml nitric acid, drip and terminate rear stirring 12 hours.Centrifugally can obtain salmon pink thick solid.
TiO 2the activation method of-MIL-100 composite: by above-mentioned salmon pink thick solid ethanol washing for several times, and solid is placed in the oven dry of 60 DEG C, baking oven, activates 3 hours subsequently in 200 DEG C of baking ovens.
TiO 2the preparation method of-MIL-100 composite water treatment film: by 500mg TiO 2-MIL-100 composite dissolves in 10ml polysulfones colloidal sol, colloidal sol is poured into cleaned glass plate surface, adopts glass bar knifing and being placed in infrared drying oven to dry, can obtain TiO 2-MIL-100-polysulfone composite membrane; Or by 500mg TiO 2-MIL-100 composite is scattered in 5mi ethanolic solution, and is poured into pvdf membrane surface, adopts glass bar that dissolution homogeneity is coated on pvdf membrane surface, then pvdf membrane is placed in baking oven dry, can obtains TiO 2-MIL-100-PVDF composite membrane.
The using method of composite water treatment film: by the film of preparation to be arranged on supporter, and be placed in cesspool, carries out fast enriching by the porous adsorbing material in film to the organic matter in sewage, by the TiO of load 2material realizes organic degraded.Meanwhile, sewage sample carries out sampling monitoring at any time, measures content of organics wherein.
The above is only the preferred embodiment of the present invention, and for those skilled in the art, under the prerequisite not departing from inventive principle, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (6)

1. a MIL-100 porous adsorbent, it is characterized in that: it is the orange red solid particle adopting hydro-thermal method to prepare, this solid particle needs first repeatedly to clean with ultra-pure water, to remove unreacted slaine, repeatedly clean with ethanol again, remove unreacted trimesic acid.
2. a MIL-100 adsorbent for high-specific surface area, good adsorption characteristic, is characterized in that: MIL-100 adsorbent according to claim 1 is needed 200 DEG C of high-temperature roasting a few hours.
3.TiO 2the synthetic method of-MIL-100 composite, is characterized in that: joined by the MIL-100 be ground into powder in ethanol (or other solvents) solution of butyl titanate, after fully stirring and evenly mixing, then drip hydrolyzate.
4.TiO 2the activation method of-MIL-100 composite, is characterized in that: gained composite need wash for several times with ethanol, and to remove unreacted butyl titanate, the composite after purification needs 200 DEG C of high-temperature roasting a few hours with activated nano TiO 2catalytic activity.
5. TiO according to claim 3 2the synthetic method of-MIL-100 composite, is characterized in that: TiO 2without any restrictions with the adding proportion of MIL-100, can need to adopt any ratio to carry out load according to research needs or practical application.
6.TiO 2the preparation method of-MIL-100 composite water treatment film, is characterized in that: TiO 2the adding proportion of-MIL-100 and polymer and TiO 2the configuration proportion of-MIL-100 suspension is without any restrictions, and the selection of membrane material is without any restrictions, can need to improve according to research needs or practical application.
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CN105056886A (en) * 2015-07-29 2015-11-18 国网山东省电力公司电力科学研究院 Absorbent for processing transformer waste oil and preparation method thereof
CN105251435A (en) * 2015-11-24 2016-01-20 天津工业大学 Preparation method of core-shell type composite material with MTN zeolite configuration
CN105498553A (en) * 2015-12-11 2016-04-20 华南理工大学 Polyvinylidene fluoride and metal-organic framework composite ultra-filtration membrane and preparation and application
CN105803760A (en) * 2016-04-07 2016-07-27 济南钛盾生物科技有限公司 Titanium dioxide textile and preparation method thereof
CN108031437A (en) * 2017-12-07 2018-05-15 苏州大学 Adsorb composite material of organic pollution and preparation method and application

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CN105056886A (en) * 2015-07-29 2015-11-18 国网山东省电力公司电力科学研究院 Absorbent for processing transformer waste oil and preparation method thereof
CN105251435A (en) * 2015-11-24 2016-01-20 天津工业大学 Preparation method of core-shell type composite material with MTN zeolite configuration
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