CN102258990A - Method for preparing light sewage treatment material - Google Patents
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- CN102258990A CN102258990A CN 201110127196 CN201110127196A CN102258990A CN 102258990 A CN102258990 A CN 102258990A CN 201110127196 CN201110127196 CN 201110127196 CN 201110127196 A CN201110127196 A CN 201110127196A CN 102258990 A CN102258990 A CN 102258990A
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Abstract
The invention relates to a method for preparing a light sewage treatment material. In the method provided by the invention, an industrial waste material is used as a raw material; the light sewage treatment material is prepared by coating a TiO2 catalyst on a glass vector with high opening porosity, thereby being beneficial to waste material utilization and environment conservation; the prepared sewage treatment material has the advantages of low density, large specific surface area, high intensity, water resistance, excellent acid-alkali resistance and simplicity in preparation process; and the prepared light sewage treatment material can be used for a sewage treatment material for large-area filtration and a sewage treatment material for the surface of a water body. The method provided by the invention can be used for effectively lowering the production cost of the sewage treatment material, is environmentally-friendly, can be used for turning waste into wealth, has obvious economic benefits and environmental friendliness benefits and has extremely wide application prospects.
Description
Technical field
The present invention relates to a kind of preparation method of sewage treating material, particularly a kind of preparation method of through hole lightweight sewage treating material.
Background technology
The industrial development in last century, population increase.Cause the rapid deterioration of present environment.Enter 21 century, the mankind are faced with many crises, and shortage of water resources is the biggest crisis that the mankind face.The water scarcity aggravation, water pollution problems is day by day seriously constantly threatening the mankind.In order to solve this crisis, the various countries scientist seeks effective method one after another and approach obtains pure water resource.It is two effective methods that desalinization and sewage disposal utilize again.
At present existing many countries have obtained pure drinking water and domestic water by desalination technology.Thereby part has solved water resources crisis.But,, there is one day seawater also can be contaminated eventually along with water pollutes aggravation if do not solve water pollution problems.The human at that time sea that will can not see vastness again, existence is on the hazard, and swimming will become the finest human memory.So it is crucial solving water pollution problems, is to take stopgap measures originally.Seeking a kind of effective water technology has become the heat subject of current scientists study.The method that is used to handle waste water has a variety of, mainly contains charcoal treatment method, aeration, anaerobic bio-treated method, embrane method, chemical oxidation treatment method and Treatment by Photocatalysis Oxidation method etc.Photocatalytic oxidation is a new method with broad development future, and its research is had profound significance.
At present, traditional method for treating water is as absorption method, Coagulation Method, activated sludge process etc.But all exist certain difficulty when these persistent organic pollutants of actual treatment, treatment effect is still undesirable.Therefore, seek a kind of economy, effective method, become the research topic that various countries environmental science worker pays much attention to these pollutants of degrading.TiO
2Photocatalytic degradation is expected to become one of method that solves this difficult problem.
TiO
2Have anti-chemistry and photoetch, stable in properties, nontoxic, catalytic activity is high, advantage such as inexpensive.Utilizing semiconductor catalyst to carry out oxidation operation is a kind of of high-level oxidation technology, and materials such as toxicity outstanding in its environmental pollution problem is big, the hydro carbons of difficult for biological degradation, halogenated aryl hydrocarbon, dyestuff, agricultural chemicals, oils have good oxygenolysis.In addition, because light-catalyzed reaction has the reaction condition gentleness, equipment is simple, secondary pollution is little, easy operating control, low concentration pollutant had advantage such as good effect of removing, be many research most active fields that present photochemical method is used for polluting control, be subjected to paying close attention to widely.In nearest 10 years, oneself obtains research the photocatalytic degradation technology of hazardous contaminant in water and the waste water (comprising organic chloride and organic compounds containing nitrogen) as a kind of deeply treatment technology.Studies show that, utilize TiO
2Carry out Treatment by Photocatalysis Oxidation, can be effectively with most of organic chlorides and multiple pesticide, rust remover, surfactant, to cause exhaustive oxidations such as color base group be CO
2, non-toxic products such as HCl and water.
In sewage disposal, mainly be with waste water by the equipment of adsorbent is housed, thereby other ions of some harmful ions in the waste water and adsorbent or group exchange and staying is removed on the adsorbent, adsorbent then recovers exchange capacity by regeneration.What application was many at present is the mineral-type adsorbent.The mineral-type adsorbent mainly contains zirconia, flyash, aluminium hydroxide, natural zeolite, modified molecular screen, activated magnesia, serpentine, activated alumina, hydroxyapatite, carry aluminium ion, bauxite, polyaluminium salts, activation aluminium, titanium dioxide, silica gel load _ titanium dioxide etc.In these inorganic adsorbents, since titanium dioxide, silica gel load titanium dioxide have anti-chemistry and photoetch, stable in properties, nontoxic, catalytic activity is high, reaction speed is fast, to organic degraded non-selectivity and easily make it advantages such as thorough mineralising, non-secondary pollution, therefore more and more widely with the application of titanium dioxide class adsorbent in wastewater treatment.
In general, a kind of good carrier should possess following condition: (1) can not have a strong impact on the absorption of film to light: (2) TiO
2And stronger physics or chemical bonding effect are arranged between the body, and this bonding action can not eliminated catalytic activity; (3) can provide higher specific surface area; (4) degradation product there is suction-operated preferably; (5) fixing physical form is arranged, be convenient to final two and be separated; (6) itself is stable high, is chemical inertness, can oxidized or reduction.Because nano-TiO
2Energy catalytic oxidation and decomposing organic matter under illumination so the used carrier great majority are inorganic material, based on the silicic acid class, are metal, active carbon etc. secondly.Doing carrier with various glasswares is the immobilized main direction of studying of photochemical catalyst, that had attempted has a glass fibre, (Li Zhijun such as Bio-Glas, sheet glass, quartz glass and soda-lime glass, Wang Hongying. the character of nano titanium oxide and application progress [J]. toothpaste industry, 2006,3:48-51; The seat Big Dipper. the effect [J] of catalyst oxidation sodium pentachlorophenol is scraped in load. environmental science, 2001,22 (1): 4; Gu Zhengrong, Chen Aiping, Dai Zhiming, etc. active carbon-nano-TiO
2The research of composite photo-catalyst air-purifying net [J]. East China University of Science's journal, 2000,26 (4): 367; Jiang Liwen. supported titanium
2Fixedly phase photocatalysis immobilization technology research [J]. Treatment of Industrial Water, 2000,20 (9): 8).Because the composition of various glass carriers, knot silica gel are because excellent adsorption is the main carrier of various catalyst cupports always.
Cheap and easy to get because of glass, itself light is had the good light transmittance energy, and be convenient to be designed to the Photoreactor of different shape, so most laboratory research sex work and explorative work with glass as carrier.Particularly, sheet glass, glass fiber mesh or cloth, hollow glass micro-ball, bead, spiral glass pipe, porous boron hydrochlorate heat resistant glass sheet (Zhao Yingna are arranged, Zhang Wenli, Wu Yinlin. the preparation of loaded nano catalysis material reaches at Application of Sewage [J]. Institutes Of Technology Of Hebei's journal, 2008,2:114), glass filter disc and optical fiber etc.Based on the research purpose difference, select multi-form glass.Because research to load technology on the sheet glass, it is the early-stage Study of the nature of glass photochemical reactor of exploitation different shape, so general experimental study carries out with the sheet glass form, lay particular emphasis on certain fixing means on glass to by the degradation effect of photocatalytic degradation thing.With bigger existence forms of specific area such as netted, cloth shape, microspheroidal, can the augmenting response area, improve reaction efficiency.Because glass surface is very smooth smooth, so to TiO
2Adhesion property relatively poor relatively., adhesion-tight good, homogeneous, the TiO that photocatalytic activity is high in its area load light transmission
2Film needs advanced technology, so still have very big researching value at present.
(P.Keim. exploitation macropore glass is as the example .Korrespondenz Abwasser of fluid bed three-dimensional growing carrier with the Anaerobic Treatment trade effluent for P.Keim, 1989,36 (6): 657-687) report is to carry out sewage disposal with graininess macropore glass as fluid bed, by actual test, higher COD clearance document does not so far appear in the newspapers in the literary composition.But the glass that is adopted in the literary composition is graininess, can't be used for the buoyancy sewage treating material of lightweight.Zhao Yingna (Zhao Yingna, Zhang Wenli, Wu Yinlin. the preparation of loaded nano catalysis material reaches at Application of Sewage [J]. Institutes Of Technology Of Hebei's journal, 2008,2:114) with Na
2O-B
2O
3-SiO
2Glass system is a foundational system, with industrial borax, boric acid, quartz, TiO
2, hydrochloric acid, ammonium chloride etc. are raw material, form to be selected in the glass phase-separating section, and add 8% TiO in foundational system
2, 1300 ℃ of fusions and be incubated 3 hours, make glass.Heat-treat then.With concentration is that the HCl of 2M carries out chemical treatment, and adds saturated NH in acid
4Cl is as buffer.92 ℃ of water-baths 4 days, used a large amount of distilled water immersions afterwards 2～3 days, be put into to dry about 50 ℃ and remember the loaded nano catalysis material.This method preparation temperature is up to 1300 ℃, and the processing time is long, and the catalysis material density that obtains is big, can not be used for the lightweight sewage treating material and use.
CN1911845A discloses a kind of through-hole foam method for glass preparation, and waste plate glass powder, manganese dioxide, di-iron trioxide and boric acid are mixed; And then add polyvinyl alcohol and the distilled water ball milling is made slurry; The plastic foam sponge is immersed in the slip, after treating in the plastic foam sponge all to immerse slips, takes out and be put on the refractory material, and move in the foaming kiln, drying, sponge burning, foaming surely steep, cool off and anneal through-hole foam glass.The present invention is raw material with the industrial waste, adds a small amount of additive, and forms agent with foam sponge as abscess, adopts the moulding of sponge cement-dipping method, has prepared through-hole foam glass.Not only help twice laid, the protection environment, and also the through-hole foam glass that makes is communicated with that the perforate porosity reaches more than 90%, light weight, high-strength, even air hole distribution.The through-hole foam glass of this method preparation can be in a large number as good sound absorption material and extraordinary filtering material (for example be used for absorb and filters HF gas or contain hydrofluoric acid liquid), still can not be used as sewage treating material.In addition, this material resistance to water, the acid-proof alkaline requirement that also do not reach sewage treating material.
CN1356270 discloses a kind of preparation method of natural bentone material used to treat sewage, the adsorption step that comprises bentonite sodium ion exchange, cetab, it is characterized in that after the displacement of natural montmorillonite sodium ion, increase following steps before the absorption of cetab: after mixing according to the ratio of 1: 2～4w/w with crystal aluminum chloride solution and sodium bentonite, vibrated 10～36 hours, centrifugal, drying is pulverized; 12～16% pore-foaming agents are joined make graininess in the bentonite, 450～600 ℃ of roastings are 1～5 hour in the Muffle furnace.The prepared bentonite sewage treatment capacity of the present invention is greatly improved, be easy to simultaneously with moisture from.But prepared sewage treating material density is big, and the porosity is low.CN1559923 and CN101428873 disclose a kind of preparation method of multifunctional fly ash sewage treating material, its preparation process is as follows: in weight portion, get 45～70 parts in flyash, aluminium salt, molysite, totally 2～15 parts of sodium polysilicates, 4～10 parts in oxidant, 10～20 parts of cement or clinkers, 5～15 parts on 20～50 order spun yarns, mixing, the gel state water that adds aforementioned thing gross mass 10～20% again, mixing, the thickness of packing into are in the rectangle module of 5～10cm, flatten, be heated to 80 ℃～160 ℃, be incubated 0.5～1.5 hour, be cooled to 20～30 ℃, air-dry, water seasoning 4～10 hours, air-dry, fragmentation, sieve product.With functions such as the flyash sewage treating material Collecting flocculation of the present invention preparation, absorption, chemical degradations in one, this material is the microporous cellular solid particle, have adsorptivity, flocculability and oxidisability, not only strengthened the absorption property of flyash, and can significantly reduce the consumption of flocculant.The prepared multifunctional fly ash sewage treating material density of this method is big, and the porosity is low, and the surface area of sample is less, can not be used for the sewage treating material of lightweight.CN1772636 discloses a kind of composite photo catalytic sewage treating material, and this material is by the semiconductor powder TiO with photocatalysis characteristic
2With powder Fe with superparamagnetism
3O
4Be composited TiO
2The semiconductor powder molar percentage is 75～90%, super-paramagnetism nano Fe
3O
4The powder molar percentage is 10～25%.Preparation TiO
2Powder coats Fe
3O
4The technology of the composite granule of particle adopts sol-gel process and hydrothermal deposition method.The TiO that will have photocatalysis characteristic
2The semiconductor powder is coated on the Fe with magnetic
3O
4Powder surface possesses photocatalysis characteristic and magnetic simultaneously thereby give advanced composite material (ACM).Add controlled alternating magnetic field, can control the semiconductor composite powder and in sewage, move, separate and reclaim.The preparation of the composite granule of this method by having photocatalysis characteristic and magnetic with the method for externally-applied magnetic field control, is carried out sewage disposal, has overcome TiO
2Powder is deposition and reduce the drawback of sewage purification ability easily, makes the use that this material can be long-term.The prepared sewage treating material of this method need be used the ferromagnetism device material is adsorbed in water surface when handling water surface and pollute, the use complex process, and the sewage treating material specific area of preparation is less.CN1798704 discloses a kind of sewage treating material, is used to handle the sewage that contains harmful substances such as arsenic, lead, cadmium, antimony, uranium, phosphorus, selenium and fluorine, and it is made of the containing oxygen iron compound that loads on the material that contains silicic acid matter fiber or phyllosilicate fiber.This processing material contacts to react with iron content acid water by the material that makes aminanthine etc. and contain the phyllosilicate fiber and obtains, and it has, and the containing oxygen iron compound is the fine structure that the sheath shape adheres on the surface of the fiber that the alkali composition reduces, silicic acid component increases in the aminanthine.By this processing material is contacted with the solution that is dissolved with poisonous metal compounds such as arsenic, remove poisonous metal.The prepared material of this method still exists specific area little, and density is big, can not handle shortcomings such as organic pollution.
CN101306838 discloses the neutral mixed crystal nano-TiO of a kind of high stable
2The preparation method of the hydrosol belongs to photocatalytic activity nanometer titanic oxide material fabricating technology field.The inventive method comprises following key step: (1). with titanium compound aqueous slkali hydrolytic precipitation.Filter washing; (2). add acid solution,, and add a certain amount of SiO at 60～100 ℃ of following dispergation
2Colloidal sol as stabilizing agent and slaine as adulterant, sustained response a period of time; (3). add pH value to 7～8 of alkali lye regulator solution; (4). filter, washing is dissolved in filter cake in a certain amount of water, disperses again, the final nano-TiO that obtains to stablize neutral mixed crystal
2Colloidal sol.The TiO of gained of the present invention
2Hydrosol spraying is easy to operate.This hydrosol can utilize solar energy to carry out sewage disposal, air cleaning, antibacterial treatment, coating film on glass processing etc.The main feature of this method is to have prepared high performance photocatalytic nanometer TiO
2, do not prepare widely used sewage treating material in the reality.CN1208670 discloses a kind of porous, Large ratio surface solid super strong acid photocatalyst, promptly with conductor oxidate TiO
2Or contain TiO
2Binary composite oxides (as: TiO
2-SiO
2, TiO
2-ZrO
2, TiO
2-Al
2O
3) be matrix, handle and make with sulfuric acid or sulfate liquor through high-temperature heat treatment.This catalyst has very strong photochemical catalytic oxidation decomposability to organic matter, and has the strong disinfecting performance.Can be applicable to room air and drink fields such as water purification, industrial waste gas and sewage disposal, flowers and fruit freshness preserving, antibiotic glass and ceramic material.The characteristics of this method are to have prepared high performance photocatalytic nanometer TiO
2, do not design widely used lightweight sewage treating material in the reality.CN201678522U sewage disposal device that utilizes the artificial swamp module, comprise surface low artificial swamp module and drowned flow artificial wet land module, by framework and inner stuffing and various wetland plant composition, described framework is the fiberglass box body, steel construction supports, and water inlet pipe and outlet pipe are set, and described inner stuffing is filled in the interior sandstone slit of framework, the main spherical light multiporous biological filtrate that adopts, described wetland plant is planted on the fertile soil of superficial layer.The present invention manages simply, does not need power consumption energy consumption equipments such as aeration, stirring, at the bottom of the operating cost of disposing of sewage, and volume is less, can make according to user's water yield, the lifting mode is installed, easy for installation, management is simple, is difficult for stopping up, the water yield is adjustable, convenient maintenance, applied widely, be particularly useful for the sanitary sewage disposal of the vast rural area of China.The sewage treating material that this method relates to is the spherical filtrate of porous, and the catalysis material that its degradable water pollutes is present in the surface of spherical filtrate.This filtering material particle is little, must be filled in the sandstone slit in the framework use complex process during use.CN101186384 discloses a kind of need not fixing, adaptable sewage biological treatment inorganic filling material, with montmorillonite powder, blowing agent, waterglass, magnesium hydroxides etc. are raw material, magnesium hydroxide and waterglass are made cementing agent, filler is easy to moulding, blowing agent can be regulated the gas porosity of filler, the proportion of control filler, manufacture craft is simple, and cost is low, can be in outdoor long-term storage, because of filler has microcellular structure, surface area is big and coarse, and the survival of suitable microorganism has strengthened the detergent power of microorganism to sanitary sewage greatly, it is effective to dispose of sewage, and easy to use, directly drop in the biochemical reactor, need not fix, impurity in the sewage, finally change into plant cell and animal protein, make sewage purification reach the tertiary treatment level, do not produce secondary pollution, reach the ecological balance by self regulating and control, be particularly useful for samll cities and towns' sewage disposal.The prepared sewage treating material of this method is difficult to be prepared into big bulk, for use in filtration treatment sewage in enormous quantities and float over water surface and dispose of sewage.In addition, this method preparation temperature is up to 1100 ℃, and at this temperature lower calcination for up to 7-9 hour, complicated process of preparation.CN1792865 discloses a kind of manufacture method of equipment for treating pollution water body, and employed carrier material is fiberglass braided material.This method can not be used to prepare the sewage treating material of lightweight.CN1884128 discloses a kind of microorganism composite carrier that is used for sewage disposal, and major ingredient is that vegetable mould, flyash, calcium silicates, kaolin, limonite are or/and zeolite; Hydrophilic substance is a diatomite; Binding agent is waterglass and/or cement; This carrier possess hydrophilic property is good, specific area big, be slightly soluble in water, nontoxic, can breed the edaphon of general metabolic function rapidly, can not produce foul smell in the process of disposing of sewage, and can denitrogenate by efficient dephosphorization, be widely used in sanitary sewage, the high concentrated organic wastewater processing engineering.The prepared sewage treating material density of this method is big, and specific area is little, can not be used to prepare the lightweight sewage treating material.
Foam glass is the novel light of a kind of superior performance, matter high-strength building material and ornament materials, and the serviceability temperature scope is subzero 196 ℃ to 450 ℃, and the A level is not fired and the same life-span of building, and thermal conductivity factor is 0.058, and moisture permeable coefficient is almost 0.Though other novel heat insulation materials emerge in an endless stream, foam glass is permanent with it, security, high reliability in fields such as low heat insulation, moistureproof engineering, sound absorptions in occupation of more and more important position.Its production is the waste solid Reuse of materials, is protection environment and the example that obtains abundant economic interests.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, the preparation method of the lightweight sewage treating material that provide a kind of lightweight, big bulk, high through-hole rate, can produce in batches.
For achieving the above object, the technical solution used in the present invention is:
The first step: the preparation of glass through hole catalyst cupport carrier
At first, waste plate glass is cleaned up, oven dry back ball milling to 250～300 orders, get glass dust behind 73% the ball milling by mass fraction then, 12% borax, 4.5% basic magnesium carbonate, 4.0% zirconia, 3.5% aluminium hydroxide and 3.0% sodium nitrate are put into ball grinder and are made batch;
Secondly, add the polyvinyl alcohol of batch quality 3～5% again in ball grinder, 0.1～0.3% carboxymethyl cellulose and 8% distilled water ball milling were made slurry in 1～3 hour;
Be 10～30kg/m with density then
3The plastic foam sponge be immersed in the slip, after treating in the plastic foam sponge all to immerse slips, take out and be put on the refractory material, and in the immigration Muffle furnace, burn till according to following calcining system: drying stage, programming rate are 1 ℃/min, are warming up to 200 ℃ and be incubated 2～3 hours from room temperature; The sponge combustion phases, programming rate is 3 ℃/min, is warming up to 400 ℃ of insulations 1～2 hour; Foam the steady bubble stage, programming rate is that 15～20 ℃/min is warming up to 830～880 ℃ of insulations 30～60 minutes; Cooling stage, cooling rate is 10 ℃/min, is cooled to 650 ℃ of insulations 40～60 minutes; Annealing stage, cooling rate is 0.5 ℃/min, is annealed to room temperature and gets glass through hole catalyst cupport carrier;
Second step: the lightweight TiO
2The preparation of catalysis sewage treating material
At first, add 50～70ml ethanol in the beaker behind cleaning, drying; Then, in beaker, add 3～5ml monoethanolamine again, and stir 5～10min; Then, add 16～18ml butyl titanate again, continue to stir 10min again; Then, dropwise add 8～10ml ethanol and 0.8～1ml distilled water again, in the dropping process, after mixing fully, two-phase adds second again, drip on one side, stir on one side, till drips of solution adds, leave standstill 20min after continue stirring 10min, stablized, even, transparent orange-yellow colloidal sol;
Once more, prepared glass through hole catalyst cupport carrier is put into orange-yellow colloidal sol, baking oven is put in taking-up after soaking 10～20min, behind insulation 5～10min under 100 ℃, after taking-up is cooled to and puts into orange-yellow colloidal sol once more after the room temperature and soak 10～20min, so repetitive coatings is 3～5 times, promptly gets and is coated with TiO
2Colloidal sol glass through hole catalyst cupport carrier;
At last, will be coated with TiO
2Colloidal sol glass through hole catalyst cupport carrier is put into Muffle furnace, is warming up to 660～750 ℃ of insulation 1～2h with the programming rate of 8 ℃/min from room temperature, closes the Muffle furnace power supply, cools to room temperature with the furnace, promptly gets lightweight TiO
2The catalysis sewage treating material.
Because the present invention is raw material with the industrial waste, by apply TiO on the glass carrier of the high perforate porosity
2Catalyst prepares the lightweight sewage treating material; not only help twice laid; the protection environment; and the sewage treating material density that makes is little, and specific area is big, the intensity height; resistance to water; resistance to acids and bases is good, and preparation technology is simple, and prepared lightweight sewage treating material can be used for bulk and filters with sewage treating material and the pollutant processing material that is used for water surface.The production cost of sewage treating material can fall in the present invention effectively, and the protection environment is turned waste into wealth, and has tangible economic benefit and environmental benefit, and application prospect is very wide.
Description of drawings
Fig. 1 is the prepared photo of lightweight sewage treating material under SEM of the embodiment of the invention 1.
The specific embodiment
Embodiment 1,
The first step: the preparation of glass through hole catalyst cupport carrier
At first, waste plate glass is cleaned up oven dry back ball milling to 300 order, get glass dust behind 73% the ball milling, 12% borax, 4.5% basic magnesium carbonate by mass fraction then, 4.0% zirconia, 3.5% aluminium hydroxide and 3.0% sodium nitrate are put into ball grinder and are made batch;
Secondly, add the polyvinyl alcohol of batch quality 3% again in ball grinder, 0.1% carboxymethyl cellulose and 8% distilled water ball milling were made slurry in 1 hour;
Be 10kg/m with density then
3The plastic foam sponge be immersed in the slip, after treating in the plastic foam sponge all to immerse slips, take out and be put on the refractory material, and in the immigration Muffle furnace, burn till according to following calcining system: drying stage, programming rate are 1 ℃/min, are warming up to 200 ℃ and be incubated 2 hours from room temperature; The sponge combustion phases, programming rate is 3 ℃/min, is warming up to 400 ℃ of insulations 1 hour; Foam the steady bubble stage, programming rate is that 15 ℃/min is warming up to 830 ℃ of insulations 30 minutes; Cooling stage, cooling rate is 10 ℃/min, is cooled to 650 ℃ of insulations 40 minutes; Annealing stage, cooling rate is 0.5 ℃/min, is annealed to room temperature and gets glass through hole catalyst cupport carrier;
Second step: the lightweight TiO
2The preparation of catalysis sewage treating material
At first, add 50ml ethanol in the beaker behind cleaning, drying; Then, in beaker, add the 3ml monoethanolamine again, and stir 5min; Then, add the 16ml butyl titanate again, continue to stir 10min again; Then, dropwise add 8ml ethanol and 0.8ml distilled water again, in the dropping process, after mixing fully, two-phase adds second again, drip on one side, stir on one side, till drips of solution adds, leave standstill 20min after continue stirring 10min, stablized, even, transparent orange-yellow colloidal sol;
Once more, prepared glass through hole catalyst cupport carrier is put into orange-yellow colloidal sol, take out behind the immersion 10min and put into baking oven, behind insulation 5min under 100 ℃, after taking-up was cooled to and puts into orange-yellow colloidal sol after the room temperature once more and soak 10min, so repetitive coatings was 3 times, promptly gets and is coated with TiO
2Colloidal sol glass through hole catalyst cupport carrier;
At last, will be coated with TiO
2Colloidal sol glass through hole catalyst cupport carrier is put into Muffle furnace, is warming up to 660 ℃ of insulation 1h with the programming rate of 8 ℃/min from room temperature, closes the Muffle furnace power supply, cools to room temperature with the furnace, promptly gets lightweight TiO
2The catalysis sewage treating material.
Formed foam glass even structure adopts reading microscope to measure the average bubble diameter in surface of sample; Adopt drainage to measure the apparent density of sample; Adopt universal testing machine to measure the rupture strength of sample.
The test correlated performance is:
Apparent density: 0.32gcm
-3
Average bubble diameter: 1.64mm;
Rupture strength: 3.1MPa;
Referring to accompanying drawing 1, by accompanying drawing as can be seen, prepared lightweight sewage treating material is a loose structure.
Embodiment 2,
The first step: the preparation of glass through hole catalyst cupport carrier
At first, waste plate glass is cleaned up oven dry back ball milling to 260 order, get glass dust behind 73% the ball milling, 12% borax, 4.5% basic magnesium carbonate by mass fraction then, 4.0% zirconia, 3.5% aluminium hydroxide and 3.0% sodium nitrate are put into ball grinder and are made batch;
Secondly, add the polyvinyl alcohol of batch quality 3% again in ball grinder, 0.2% carboxymethyl cellulose and 8% distilled water ball milling were made slurry in 1.2 hours;
Be 12kg/m with density then
3The plastic foam sponge be immersed in the slip, after treating in the plastic foam sponge all to immerse slips, take out and be put on the refractory material, and in the immigration Muffle furnace, burn till according to following calcining system: drying stage, programming rate are 1 ℃/min, are warming up to 200 ℃ and be incubated 2.1 hours from room temperature; The sponge combustion phases, programming rate is 3 ℃/min, is warming up to 400 ℃ of insulations 1.5 hours; Foam the steady bubble stage, programming rate is that 16 ℃/min is warming up to 840 ℃ of insulations 30 minutes; Cooling stage, cooling rate is 10 ℃/min, is cooled to 650 ℃ of insulations 50 minutes; Annealing stage, cooling rate is 0.5 ℃/min, is annealed to room temperature and gets glass through hole catalyst cupport carrier;
Second step: the lightweight TiO
2The preparation of catalysis sewage treating material
At first, add 60ml ethanol in the beaker behind cleaning, drying; Then, in beaker, add the 4ml monoethanolamine again, and stir 10min; Then, add the 18ml butyl titanate again, continue to stir 10min again; Then, dropwise add 10ml ethanol and 1ml distilled water again, in the dropping process, after mixing fully, two-phase adds second again, drip on one side, stir on one side, till drips of solution adds, leave standstill 20min after continue stirring 10min, stablized, even, transparent orange-yellow colloidal sol;
Once more, prepared glass through hole catalyst cupport carrier is put into orange-yellow colloidal sol, take out behind the immersion 20min and put into baking oven, behind insulation 10min under 100 ℃, after taking-up was cooled to and puts into orange-yellow colloidal sol after the room temperature once more and soak 20min, so repetitive coatings was 3 times, promptly gets and is coated with TiO
2Colloidal sol glass through hole catalyst cupport carrier;
At last, will be coated with TiO
2Colloidal sol glass through hole catalyst cupport carrier is put into Muffle furnace, is warming up to 680 ℃ of insulation 1h with the programming rate of 8 ℃/min from room temperature, closes the Muffle furnace power supply, cools to room temperature with the furnace, promptly gets lightweight TiO
2The catalysis sewage treating material.
Formed foam glass even structure adopts reading microscope to measure the average bubble diameter in surface of sample; Adopt drainage to measure the apparent density of sample; Adopt universal testing machine to measure the rupture strength of sample.
The test correlated performance is:
Apparent density: 0.36gcm
-3
Average bubble diameter: 1.54mm;
Rupture strength: 3.4MPa.
Embodiment 3,
The first step: the preparation of glass through hole catalyst cupport carrier
At first, waste plate glass is cleaned up oven dry back ball milling to 280 order, get glass dust behind 73% the ball milling, 12% borax, 4.5% basic magnesium carbonate by mass fraction then, 4.0% zirconia, 3.5% aluminium hydroxide and 3.0% sodium nitrate are put into ball grinder and are made batch;
Secondly, add the polyvinyl alcohol of batch quality 4% again in ball grinder, 0.2% carboxymethyl cellulose and 8% distilled water ball milling were made slurry in 3 hours;
Be 30kg/m with density then
3The plastic foam sponge be immersed in the slip, after treating in the plastic foam sponge all to immerse slips, take out and be put on the refractory material, and in the immigration Muffle furnace, burn till according to following calcining system: drying stage, programming rate are 1 ℃/min, are warming up to 200 ℃ and be incubated 3 hours from room temperature; The sponge combustion phases, programming rate is 3 ℃/min, is warming up to 400 ℃ of insulations 2 hours; Foam the steady bubble stage, programming rate is that 20 ℃/min is warming up to 850 ℃ of insulations 30 minutes; Cooling stage, cooling rate is 10 ℃/min, is cooled to 650 ℃ of insulations 60 minutes; Annealing stage, cooling rate is 0.5 ℃/min, is annealed to room temperature and gets glass through hole catalyst cupport carrier;
Second step: the lightweight TiO
2The preparation of catalysis sewage treating material
At first, add 70ml ethanol in the beaker behind cleaning, drying; Then, in beaker, add the 5ml monoethanolamine again, and stir 8min; Then, add the 16.5ml butyl titanate again, continue to stir 10min again; Then, dropwise add 10ml ethanol and 1ml distilled water again, in the dropping process, after mixing fully, two-phase adds second again, drip on one side, stir on one side, till drips of solution adds, leave standstill 20min after continue stirring 10min, stablized, even, transparent orange-yellow colloidal sol;
Once more, prepared glass through hole catalyst cupport carrier is put into orange-yellow colloidal sol, take out behind the immersion 15min and put into baking oven, behind insulation 10min under 100 ℃, after taking-up was cooled to and puts into orange-yellow colloidal sol after the room temperature once more and soak 15min, so repetitive coatings was 4 times, promptly gets and is coated with TiO
2Colloidal sol glass through hole catalyst cupport carrier;
At last, will be coated with TiO
2Colloidal sol glass through hole catalyst cupport carrier is put into Muffle furnace, is warming up to 700 ℃ of insulation 2h with the programming rate of 8 ℃/min from room temperature, closes the Muffle furnace power supply, cools to room temperature with the furnace, promptly gets lightweight TiO
2The catalysis sewage treating material.
Formed foam glass even structure adopts reading microscope to measure the average bubble diameter in surface of sample; Adopt drainage to measure the apparent density of sample; Adopt universal testing machine to measure the rupture strength of sample.
The test correlated performance is:
Apparent density: 0.31gcm
-3
Average bubble diameter: 1.74mm;
Rupture strength: 2.2MPa.
Embodiment 4,
The first step: the preparation of glass through hole catalyst cupport carrier
At first, waste plate glass is cleaned up oven dry back ball milling to 280 order, get glass dust behind 73% the ball milling, 12% borax, 4.5% basic magnesium carbonate by mass fraction then, 4.0% zirconia, 3.5% aluminium hydroxide and 3.0% sodium nitrate are put into ball grinder and are made batch;
Secondly, add the polyvinyl alcohol of batch quality 4% again in ball grinder, 0.2% carboxymethyl cellulose and 8% distilled water ball milling were made slurry in 2 hours;
Be 20kg/m with density then
3The plastic foam sponge be immersed in the slip, after treating in the plastic foam sponge all to immerse slips, take out and be put on the refractory material, and in the immigration Muffle furnace, burn till according to following calcining system: drying stage, programming rate are 1 ℃/min, are warming up to 200 ℃ and be incubated 2.5 hours from room temperature; The sponge combustion phases, programming rate is 3 ℃/min, is warming up to 400 ℃ of insulations 1 hour; Foam the steady bubble stage, programming rate is that 18 ℃/min is warming up to 860 ℃ of insulations 40 minutes; Cooling stage, cooling rate is 10 ℃/min, is cooled to 650 ℃ of insulations 60 minutes; Annealing stage, cooling rate is 0.5 ℃/min, is annealed to room temperature and gets glass through hole catalyst cupport carrier;
Second step: the lightweight TiO
2The preparation of catalysis sewage treating material
At first, add 70ml ethanol in the beaker behind cleaning, drying; Then, in beaker, add the 5ml monoethanolamine again, and stir 8min; Then, add the 17.5ml butyl titanate again, continue to stir 10min again; Then, dropwise add 8.5ml ethanol and 0.9ml distilled water again, in the dropping process, after mixing fully, two-phase adds second again, drip on one side, stir on one side, till drips of solution adds, leave standstill 20min after continue stirring 10min, stablized, even, transparent orange-yellow colloidal sol;
Once more, prepared glass through hole catalyst cupport carrier is put into orange-yellow colloidal sol, take out behind the immersion 10min and put into baking oven, behind insulation 8min under 100 ℃, after taking-up was cooled to and puts into orange-yellow colloidal sol after the room temperature once more and soak 10min, so repetitive coatings was 4 times, promptly gets and is coated with TiO
2Colloidal sol glass through hole catalyst cupport carrier;
At last, will be coated with TiO
2Colloidal sol glass through hole catalyst cupport carrier is put into Muffle furnace, is warming up to 690 ℃ of insulation 1.5h with the programming rate of 8 ℃/min from room temperature, closes the Muffle furnace power supply, cools to room temperature with the furnace, promptly gets lightweight TiO
2The catalysis sewage treating material.
Formed foam glass even structure adopts reading microscope to measure the average bubble diameter in surface of sample; Adopt drainage to measure the apparent density of sample; Adopt universal testing machine to measure the rupture strength of sample.
The test correlated performance is:
Apparent density: 0.31gcm
-3
Average bubble diameter: 1.71mm;
Rupture strength: 2.6MPa.
Embodiment 5,
The first step: the preparation of glass through hole catalyst cupport carrier
At first, waste plate glass is cleaned up oven dry back ball milling to 270 order, get glass dust behind 73% the ball milling, 12% borax, 4.5% basic magnesium carbonate by mass fraction then, 4.0% zirconia, 3.5% aluminium hydroxide and 3.0% sodium nitrate are put into ball grinder and are made batch;
Secondly, add the polyvinyl alcohol of batch quality 5% again in ball grinder, 0.3% carboxymethyl cellulose and 8% distilled water ball milling were made slurry in 2.5 hours;
Be 25kg/m with density then
3The plastic foam sponge be immersed in the slip, after treating in the plastic foam sponge all to immerse slips, take out and be put on the refractory material, and in the immigration Muffle furnace, burn till according to following calcining system: drying stage, programming rate are 1 ℃/min, are warming up to 200 ℃ and be incubated 3 hours from room temperature; The sponge combustion phases, programming rate is 3 ℃/min, is warming up to 400 ℃ of insulations 2 hours; Foam the steady bubble stage, programming rate is that 17 ℃/min is warming up to 880 ℃ of insulations 60 minutes; Cooling stage, cooling rate is 10 ℃/min, is cooled to 650 ℃ of insulations 55 minutes; Annealing stage, cooling rate is 0.5 ℃/min, is annealed to room temperature and gets glass through hole catalyst cupport carrier;
Second step: the lightweight TiO
2The preparation of catalysis sewage treating material
At first, add 65ml ethanol in the beaker behind cleaning, drying; Then, in beaker, add the 5ml monoethanolamine again, and stir 9min; Then, add the 17ml butyl titanate again, continue to stir 10min again; Then, dropwise add 9ml ethanol and 0.9ml distilled water again, in the dropping process, after mixing fully, two-phase adds second again, drip on one side, stir on one side, till drips of solution adds, leave standstill 20min after continue stirring 10min, stablized, even, transparent orange-yellow colloidal sol;
Once more, prepared glass through hole catalyst cupport carrier is put into orange-yellow colloidal sol, take out behind the immersion 18min and put into baking oven, behind insulation 9min under 100 ℃, after taking-up was cooled to and puts into orange-yellow colloidal sol after the room temperature once more and soak 18min, so repetitive coatings was 5 times, promptly gets and is coated with TiO
2Colloidal sol glass through hole catalyst cupport carrier;
At last, will be coated with TiO
2Colloidal sol glass through hole catalyst cupport carrier is put into Muffle furnace, is warming up to 720 ℃ of insulation 1.5h with the programming rate of 8 ℃/min from room temperature, closes the Muffle furnace power supply, cools to room temperature with the furnace, promptly gets lightweight TiO
2The catalysis sewage treating material.
Formed foam glass even structure adopts reading microscope to measure the average bubble diameter in surface of sample; Adopt drainage to measure the apparent density of sample; Adopt universal testing machine to measure the rupture strength of sample.
The test correlated performance is:
Apparent density: 0.38gcm
-3
Average bubble diameter: 1.79mm;
Rupture strength: 2.1MPa.
Embodiment 6,
The first step: the preparation of glass through hole catalyst cupport carrier
At first, waste plate glass is cleaned up oven dry back ball milling to 250 order, get glass dust behind 73% the ball milling, 12% borax, 4.5% basic magnesium carbonate by mass fraction then, 4.0% zirconia, 3.5% aluminium hydroxide and 3.0% sodium nitrate are put into ball grinder and are made batch;
Secondly, add the polyvinyl alcohol of batch quality 3.5% again in ball grinder, 0.3% carboxymethyl cellulose and 8% distilled water ball milling were made slurry in 1.5 hours;
Be 16kg/m with density then
3The plastic foam sponge be immersed in the slip, after treating in the plastic foam sponge all to immerse slips, take out and be put on the refractory material, and in the immigration Muffle furnace, burn till according to following calcining system: drying stage, programming rate are 1 ℃/min, are warming up to 200 ℃ and be incubated 2 hours from room temperature; The sponge combustion phases, programming rate is 3 ℃/min, is warming up to 400 ℃ of insulations 1.5 hours; Foam the steady bubble stage, programming rate is that 19 ℃/min is warming up to 870 ℃ of insulations 50 minutes; Cooling stage, cooling rate is 10 ℃/min, is cooled to 650 ℃ of insulations 45 minutes; Annealing stage, cooling rate is 0.5 ℃/min, is annealed to room temperature and gets glass through hole catalyst cupport carrier;
Second step: the lightweight TiO
2The preparation of catalysis sewage treating material
At first, add 55ml ethanol in the beaker behind cleaning, drying; Then, in beaker, add the 4.5ml monoethanolamine again, and stir 7min; Then, add the 18ml butyl titanate again, continue to stir 10min again; Then, dropwise add 9.5ml ethanol and 0.8ml distilled water again, in the dropping process, after mixing fully, two-phase adds second again, drip on one side, stir on one side, till drips of solution adds, leave standstill 20min after continue stirring 10min, stablized, even, transparent orange-yellow colloidal sol;
Once more, prepared glass through hole catalyst cupport carrier is put into orange-yellow colloidal sol, take out behind the immersion 13min and put into baking oven, behind insulation 7min under 100 ℃, after taking-up was cooled to and puts into orange-yellow colloidal sol after the room temperature once more and soak 13min, so repetitive coatings was 5 times, promptly gets and is coated with TiO
2Colloidal sol glass through hole catalyst cupport carrier;
At last, will be coated with TiO
2Colloidal sol glass through hole catalyst cupport carrier is put into Muffle furnace, is warming up to 750 ℃ of insulation 1h with the programming rate of 8 ℃/min from room temperature, closes the Muffle furnace power supply, cools to room temperature with the furnace, promptly gets lightweight TiO
2The catalysis sewage treating material.
Formed foam glass even structure adopts reading microscope to measure the average bubble diameter in surface of sample; Adopt drainage to measure the apparent density of sample; Adopt universal testing machine to measure the rupture strength of sample.
The test correlated performance is:
Apparent density: 0.36gcm
-3
Average bubble diameter: 1.67mm;
Rupture strength: 1.9MPa.
Because the present invention is raw material with the industrial waste, by apply TiO on the glass carrier of the high perforate porosity
2Catalyst prepares the lightweight sewage treating material, not only helps twice laid, the protection environment, and also the sewage treating material density that makes is little, and specific area is big, the intensity height, resistance to water, resistance to acids and bases is good, and preparation technology is simple.Prepared lightweight sewage treating material can be used for bulk and filters with sewage treating material and the pollutant processing material that is used for water surface.Thereby having considerable economic and social benefit, application prospect is very wide.
Claims (1)
1. the preparation method of a lightweight sewage treating material is characterized in that:
The first step: the preparation of glass through hole catalyst cupport carrier
At first, waste plate glass is cleaned up, oven dry back ball milling to 250～300 orders, get glass dust behind 73% the ball milling by mass fraction then, 12% borax, 4.5% basic magnesium carbonate, 4.0% zirconia, 3.5% aluminium hydroxide and 3.0% sodium nitrate are put into ball grinder and are made batch;
Secondly, add the polyvinyl alcohol of batch quality 3～5% again in ball grinder, 0.1～0.3% carboxymethyl cellulose and 8% distilled water ball milling were made slurry in 1～3 hour;
Be 10～30kg/m with density then
3The plastic foam sponge be immersed in the slip, after treating in the plastic foam sponge all to immerse slips, take out and be put on the refractory material, and in the immigration Muffle furnace, burn till according to following calcining system: drying stage, programming rate are 1 ℃/min, are warming up to 200 ℃ and be incubated 2～3 hours from room temperature; The sponge combustion phases, programming rate is 3 ℃/min, is warming up to 400 ℃ of insulations 1～2 hour; Foam the steady bubble stage, programming rate is that 15～20 ℃/min is warming up to 830～880 ℃ of insulations 30～60 minutes; Cooling stage, cooling rate is 10 ℃/min, is cooled to 650 ℃ of insulations 40～60 minutes; Annealing stage, cooling rate is 0.5 ℃/min, is annealed to room temperature and gets glass through hole catalyst cupport carrier;
Second step: the lightweight TiO
2The preparation of catalysis sewage treating material
At first, add 50～70ml ethanol in the beaker behind cleaning, drying; Then, in beaker, add 3～5ml monoethanolamine again, and stir 5～10min; Then, add 16～18ml butyl titanate again, continue to stir 10min again; Then, dropwise add 8～10ml ethanol and 0.8～1ml distilled water again, in the dropping process, after mixing fully, two-phase adds second again, drip on one side, stir on one side, till drips of solution adds, leave standstill 20min after continue stirring 10min, stablized, even, transparent orange-yellow colloidal sol;
Once more, prepared glass through hole catalyst cupport carrier is put into orange-yellow colloidal sol, baking oven is put in taking-up after soaking 10～20min, behind insulation 5～10min under 100 ℃, after taking-up is cooled to and puts into orange-yellow colloidal sol once more after the room temperature and soak 10～20min, so repetitive coatings is 3～5 times, promptly gets and is coated with TiO
2Colloidal sol glass through hole catalyst cupport carrier;
At last, will be coated with TiO
2Colloidal sol glass through hole catalyst cupport carrier is put into Muffle furnace, is warming up to 660～750 ℃ of insulation 1～2h with the programming rate of 8 ℃/min from room temperature, closes the Muffle furnace power supply, cools to room temperature with the furnace, promptly gets lightweight TiO
2The catalysis sewage treating material.
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| CN201110127196A CN102258990B (en) | 2011-05-17 | 2011-05-17 | Method for preparing light sewage treatment material |
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| CN103877694A (en) * | 2014-03-13 | 2014-06-25 | 江苏大学 | Method for carrying out visible light anaerobic degradation on organic pollutants mediated by TiO2 nano materials |
| CN104874343A (en) * | 2015-05-22 | 2015-09-02 | 周末 | Preparation method for nano-titanium dioxide glass fiber composite material |
| CN104998466A (en) * | 2015-08-20 | 2015-10-28 | 崔学烈 | Light filtration medium for water treatment and preparation method and application thereof |
| CN105126786A (en) * | 2015-08-07 | 2015-12-09 | 哈尔滨工业大学 | Preparation method, desorption method and applications of carbon nano-tube/polyaniline composite adsorption material with characteristic of easy lightweight separation |
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| CN104998466A (en) * | 2015-08-20 | 2015-10-28 | 崔学烈 | Light filtration medium for water treatment and preparation method and application thereof |
| CN108212138A (en) * | 2016-12-09 | 2018-06-29 | 北京有色金属研究总院 | A kind of preparation process of lanthanum and graphene oxide codope lightweight catalysis material |
| CN107935388A (en) * | 2017-11-24 | 2018-04-20 | 任合超 | A kind of the pottery fish jar and its preparation process of energy deodorizing antibiotic |
| CN109231841A (en) * | 2018-10-22 | 2019-01-18 | 深圳市优力凯环保生物技术有限公司 | A kind of foamed glass material and preparation method thereof reducing water quality fluorine element index |
| CN110533244A (en) * | 2019-08-28 | 2019-12-03 | 重庆大学 | A kind of step dam Optimization Scheduling, system and computer readable storage medium |
| CN112028497A (en) * | 2020-08-14 | 2020-12-04 | 河北迪纳兴科生物科技有限公司 | Integrated circulating system for producing pore-size-controllable nano porous glass |
| CN113321385A (en) * | 2021-06-30 | 2021-08-31 | 陈宁 | Method for reducing tail water COD value in activated sludge process sewage treatment system |
| CN114870825A (en) * | 2022-05-12 | 2022-08-09 | 江苏晶瑞特环保新材料有限公司 | Preparation and application method of novel photocatalytic glass pumice |
| CN114956635A (en) * | 2022-06-15 | 2022-08-30 | 清华珠三角研究院 | Sludge pretreatment method and production system and method for manufacturing recycled aggregate |
| CN115531978A (en) * | 2022-09-14 | 2022-12-30 | 江苏永冠给排水设备有限公司 | Preparation method and application of novel suspended lightweight filter material for drinking water treatment |
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