CN106607015A - Nano titanium dioxide photocatalyst with double-particle size distribution and preparation method thereof - Google Patents

Nano titanium dioxide photocatalyst with double-particle size distribution and preparation method thereof Download PDF

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CN106607015A
CN106607015A CN201611117008.1A CN201611117008A CN106607015A CN 106607015 A CN106607015 A CN 106607015A CN 201611117008 A CN201611117008 A CN 201611117008A CN 106607015 A CN106607015 A CN 106607015A
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titanium dioxide
nano titanium
dioxide photocatalyst
photocatalyst
double
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CN106607015B (en
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彭锋
易正求
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Guangzhou City Yi Environmental Protection Technology Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063Titanium; Oxides or hydroxides thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/40Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts

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  • Organic Chemistry (AREA)
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Abstract

The invention provides a nano titanium dioxide photocatalyst with double-particle size distribution and a preparation method thereof. The method includes: dissolving an organic titanate in an alcohol solution, adding an aqueous solution of polyacrylic acid and polyvinylpyrrolidone dropwise under stirring to prepare a transparent titanium dioxide sol; then adding a commodity nano titanium dioxide powder and carrying out ultrasonic stirring to obtain titanium dioxide colloids from transparent to translucent; and finally conducting spray drying, thus obtaining the nano titanium dioxide photocatalyst with double-particle size distribution. The titanium dioxide photocatalyst prepared by the method provided by the invention has no need for adding any surfactant or dispersant during use, by water adding and stirring, a high-stability nano titanium dioxide photocatalyst spray solution can be prepared, and can be placed stably for more than 6 months. The catalyst provided by the invention has high activity on photocatalytic degradation of organic matters under sunlight, and the degradation rate is 40% higher than that the existing commodity nano titanium dioxide P25.

Description

A kind of nano titanium dioxide photocatalyst of pair of particle diameter distribution and preparation method thereof
Technical field
The present invention relates to nano titanium dioxide photocatalyst of a kind of pair of particle diameter distribution and preparation method thereof, the photocatalyst The nano titanium oxide spray coating liquor of stable dispersion directly can be configured in the application with water, and stably can be preserved more than 6 months, The photocatalytic activity of nano titanium oxide more existing than existing market is high simultaneously.Photocatalyst prepared by the method is in environmental improvement It is middle to promote expected by the economic benefit for having produced and environmental benefit, belong to environmentally conscious materials field.
Background technology
So-called photocatalyst, is exactly the irradiation through light, can promote the material of chemical reaction.As photocatalyst can be with Process air in or water in extremely low concentration harmful chemical, harmful organic substance can be completely decomposed into water and carbon dioxide, And itself will not decompose release harmful substance, therefore it is extremely excellent surrounding purifying material.With the development of modern economy, environment Also more and more higher is required, photocatalyst is received more and more attention, in smelly eliminating, sterilization, antibacterial, antifouling and removing harmful substance Etc. the application prospect that shows of aspect.At present, the material that can be used as photocatalyst has many kinds, wherein nanometer titanium dioxide Titanium, due to stable in properties, nontoxic, and efficient photocatalytic activity, is photocatalyst the most frequently used at present, and existing market On the photocatalyst that commonly gets the nod.
The nano titanium dioxide photocatalyst sold in the market mainly has two types, a kind of pressed powder, performance The Nano titanium dioxide P25 that most preferably goldschmidt chemical corporation of common accreditation is produced on market, another is nano-silica Change titanium dispersion liquid.For nano titanium oxide pressed powder product, to be disperseed in the application, and it is a crucial skill to disperse Art, and be most difficult at present, various dispersants will be added, and applicable dispersion be obtained using various dispersing apparatus, typically User, the technical formula and special equipment for not having specialty are extremely difficult to stable dispersion liquid, so domestic consumer is rarely employed, Sell after the environmental protection company dispersion for being all specialty, but long-time stability still do not solved (can be layered within 1 month) after disperseing at present, Can not keep for a long time and transport.For nano titanium oxide dispersion product, except above-mentioned employing nanoscale titanium dioxide Outside the dispersion liquid that titanium is processed into, also one kind is Nano titanium dioxide colloidal sol, and its stability can be solved, but concentration is low (big It is many below 1%), content has substantial amounts of organic solvent, and cost of transportation is high, it is often more important that due to colloidal sol crystallinity it is poor, without Overheating Treatment is directly using the photocatalysis performance of the product than relatively low.
In order to solve these problems, both at home and abroad in terms of nano titanium oxide dispersant and Nano titanium dioxide colloidal sol all Exploitation is conducted extensive research, the Chinese patent containing titanium dioxide in title there are 508 disclosed in 2014,2015 579 are reached disclosed in year.As Chinese invention patent (publication number CN200310112124.0) discloses a kind of nanometer titanium dioxide The process for dispersing of titanium valve body, it is characterised in that nano-titanium dioxide powder is dissolved in and with the addition of the molten of surfactant and dispersant In agent, surfactant is cationic cellulose, sodium hexameta phosphate, dodecylbenzene sodium sulfonate, isobutyl group sodium sulfonate or double hard Ester acid PVOH ether;Dispersant is Disperbyk-034, Disperbyk-190, Disperbyk-183, ROHM AND HAAS 890, sieve Door Haas 1124, ROHM AND HAAS 1288, ROHM AND HAAS 731A, NC890 and LOPON895;This be by solvent, surfactant and The dispersion that dispersant is constituted.It is adapted to carry out dispersion use to nano-titanium dioxide powder material, its formula is all compared with technique It is more complicated.For example, Chinese invention patent (publication number CN201510974495.2) discloses a kind of inorganic water white transparency nanometer two The preparation method of titania photocatalyst, using titanium tetrachloride by low temperature hydrolysis, with prepared slurry in low temperature ammonia, then passes through High speed centrifuge carries out solid-liquid separation, and deionized water repeated washing, centrifugation;It is molten by hydrogen peroxide low-temperature oxidation Solution, (170-190 DEG C) of high temperature circulate complexation, water white transparency nanometer titanium dioxide are obtained using high intensity (254nm) ultraviolet catalytic Titanium photocatalyst (colloidal sol), the catalyst energy catalytic degradation Organic substance, purifies the air of a room, and improves IAQ (indoor air quality).The party Method prepares complexity, and product remains the colloidal sol of low concentration.Chinese invention patent (publication number CN201510036659.7) is also disclosed A kind of preparation method of monodisperse nano-titanium dioxide colloidal sol, using titanium tetrachloride and butyl titanate simultaneously as titanium source, with four The hydrochloric acid that titanium chloride hydrolysis is obtained is used as catalyst, and the product that hydrolysis is obtained is anti-as nucleus induction butyl titanate hydrolysis Should, solid content is obtained by the time of the ratio for controlling titanium tetrachloride, butyl titanate and deionized water, stirring and heating adjustable Stable titanium colloidal sol.The method product remains the colloidal sol of low concentration, does not prepare redispersible pressed powder.
It is an object of the invention to adopt condition relatively mild, the industrial method easily realized is prepared a kind of easily steady Fixed scattered nano titanium dioxide photocatalyst, the nano titanium oxide is a kind of pressed powder with collosol property, is being answered The nano titanium oxide spray coating liquor of stable dispersion directly can be configured with water, and stably can be preserved more than 6 months;Simultaneously Under sunlight, the activity of its photocatalytic activity nano titanium oxide P25 more best than existing market increases, based on this, We design the nano titanium oxide of a kind of pair of particle diameter distribution, expand absorption of the titanium dioxide to solar spectrum, strengthen activity, full The requirement of sufficient field of environmental improvement application.Up till now for this purpose, not reporting that this high activity with collosol property is received both at home and abroad Rice titanium dioxide solids powder.
The photocatalyst of the invention, with storage than colloidal sol conveniently, low cost, no solvent, long shelf-life are safe for its transport Property is good;The not only nano titanium dioxide photocatalyst of the related all commercially available invention of company but also domestic consumer of environmental area, Convenient configuration is used, and the catalyst is promoted the use of expected by the economic benefit for having produced and environmental benefit in environmental area.
The content of the invention
It is an object of the invention to adopt condition relatively mild, the industrial method easily realized is prepared a kind of easily steady Fixed dispersion and activity are got back the nano titanium dioxide photocatalyst of raising, and the nano titanium oxide in the application can be straight The nano titanium oxide spray coating liquor that stable dispersion is configured with water is connect, and stably can be preserved more than 6 months, while comparing existing market The activity of existing nano titanium oxide is high, meets the requirement of field of environmental improvement application.
Nano titanium dioxide photocatalyst of double particle diameter distributions of the present invention and preparation method thereof, it is characterised in that include Following steps:
(1) organic titanate of certain mass is dissolved in alcoholic solution, unlatching is stirred and is added dropwise over a certain amount of poly- The aqueous solution of acrylic acid and polyvinylpyrrolidone, be hydrolyzed at 30~60 DEG C 2~6h of reaction, obtains transparent titanium dioxide Titanium colloidal sol;
(2) given commodity nano titanium dioxide powder is added to into (1) described colloidal sol, 0.5~3h of ultrasonic agitation is obtained To transparent to translucent colloidal tio 2;
(3) complex that (2) obtain is spray-dried, the nano titanium dioxide photocatalyst of double particle diameter distributions is obtained Powder.
In the step (1), it is characterised in that organic titanate:Alcohol:Polyacrylic acid:Polyvinylpyrrolidone:The matter of water Measuring ratio is:100:100~800:1~10:0.1~5:100~1000.Wherein, organic titanate is butyl titanate or titanium Sour four isopropyl esters;Alcohol is ethanol, propanol, ethylene glycol.
In the step (2), it is characterised in that commodity nano titanium oxide addition with the mass ratio of organic titanate is 10~100:100;Preferred commodity nano titanium oxide is market flow-through P25 titanium dioxide.
In the step (3), it is characterised in that be dried using conventional pressure spray dryer device, pressure 1-10Mpa, heat Air is dried medium, temperature 150-250 DEG C.
Compared with prior art, the present invention has the advantage that and effect:
1st, preparation condition of the present invention is relatively mild, industrial easily to realize, its preparation method have obvious novelty with Advance, shows in terms of three, and one is in prepared by colloidal sol to substitute general mineral acid (hydrochloric acid, nitric acid) using polyacrylic acid, Not only prevent corrosivity and the hazardness of subsequent product, at the same polyacrylic acid coordinate together with polyvinylpyrrolidone can conduct Good stable dispersant;Two is the addition commodity nano titanium oxide in colloidal sol, can induce the crystallization of colloidal sol, increases in colloidal sol The concentration of nano titanium oxide, while further with the stable dispersant cladding commodity nano titanium oxide in colloidal sol;Three are To colloid using being spray-dried, it is to avoid reunion of the general heat treatment to material, the method not only be easy to reclaim by solvent, Er Qiebao Dispersion and the cladding of nano titanium oxide in colloid have been demonstrate,proved, and guarantee have been provided for the follow-up application of dispersion again.
2nd, titanium dioxide optical catalyst prepared by the present invention has special application advantage, no longer needs addition in use Any surfactant and dispersant, add water and the nano titanium dioxide photocatalyst spray coating liquor of high stable are prepared by stirring, and two The mass concentration of titanium oxide can regulate and control in 0.1~5% scope, and stably can place more than 6 months with good stability.
3rd, the application effect that titanium dioxide optical catalyst prepared by the present invention has had, due to mean diameter 5-10nm With double particle diameter distributions of 25-30nm, such as Fig. 1-5, the Photocatalytic activity improved under sunlight to Organic substance that can be maximum, its Degradation rate improves more than 40% than existing goods P25 nano titanium oxides.
Description of the drawings
Fig. 1 is the high resolution scanning of the nano titanium dioxide photocatalyst of double particle diameter distributions prepared by present example 1 Electromicroscopic photograph (SEM) figure.As illustrated, small particle average out to 6nm, big particle diameter average out to 25nm.
Fig. 2 is the high resolution scanning of the nano titanium dioxide photocatalyst of double particle diameter distributions prepared by present example 2 Electromicroscopic photograph (SEM) figure.As illustrated, small particle average out to 8nm, big particle diameter average out to 28nm.
Fig. 3 is the particle statistic result of the nano titanium dioxide photocatalyst of double particle diameter distributions prepared by present example 4 Figure, little particle mean diameter are 10nm, and bulky grain mean diameter is 30nm.
Fig. 4 is the particle statistic result of the nano titanium dioxide photocatalyst of double particle diameter distributions prepared by present example 5 Figure, little particle mean diameter are 5nm, and bulky grain mean diameter is 25nm.
Specific embodiment
Invention is described in further detail below by way of specific embodiment, but the invention is not restricted to following examples.
Embodiment 1
Add 100g butyl titanates, 100g ethanol to stir in the reactor, control temperature 50 C, low whipping speed Under the conditions of 500-1000 rev/min, 1g polyacrylic acid, 1g polyvinylpyrrolidones, the mixed solution of 500g water, body are slowly added into Four ester of metatitanic acid in system:Ethanol:Polyacrylic acid:Polyvinylpyrrolidone:Mass ratio=100 of water:100:1:1:500;Constant temperature is stirred Vitreosol is formed after mixing reaction 3h, 30g commodity nano titanium oxide P25 are added, starts ultrasonic agitation, continue 1h, formed Transparent colloid;The colloid for obtaining is obtained at pressure 1MPa, 250 DEG C of hot-air using conventional pressure spray dryer device The nano titanium dioxide photocatalyst of double particle diameter distributions, as shown in figure 1, small particle average out to 6nm, big particle diameter average out to 25nm.
Application effect:Catalyst obtained in 10g is taken, plus 990g pure water stirring 0.5h can be prepared by the 1% of stable dispersion Nano titanium dioxide photocatalyst spray coating liquor, placement will not be layered for 8 months.The catalyst of preparation photocatalysis drop under sunlight Organic methyl orange in Xie Shui, under the conditions of catalyst amount 1g/L, methyl orange concentration 20mg/L, reacts 3h, and degradation rate is 88.5%;The degradation rate of commodity nano titanium oxide P25 is 54.2% under the same conditions, and activity improves 63.3%.
Embodiment 2
Add 100g tetraisopropyl titanates, 400g propanol to stir in the reactor, control 30 DEG C of temperature, in stirring speed Under the conditions of 500-1000 rev/min of degree, 10g polyacrylic acid is slowly added into, 0.1g polyvinylpyrrolidones, the mixing of 400g water are molten Liquid, four ester of metatitanic acid in system:Ethanol:Polyacrylic acid:Polyvinylpyrrolidone:Mass ratio=100 of water:400:10:0.1: 400;Vitreosol is formed after constant temperature stirring reaction 5h, 10g commodity nano titanium oxide P25 are added, is started ultrasonic agitation, is held Continuous 3h, forms transparent colloid;Pressure spray dryer device of the colloid for obtaining using routine, in pressure 5MPa, hot-air 200 The nano titanium dioxide photocatalyst of double particle diameter distributions is obtained at DEG C, as shown in Fig. 2 small particle average out to 8nm, big particle diameter is average For 28nm.
Application effect:Catalyst obtained in 50g is taken, plus 950g pure water stirring 0.5h can be prepared by the 5% of stable dispersion Nano titanium dioxide photocatalyst spray coating liquor, placement will not be layered for 6 months.The catalyst of preparation photocatalysis drop under sunlight Solution air Organic substance formaldehyde, in catalyst amount 0.1g/M3, concentration of formaldehyde 10mg/M3Under the conditions of, 2h is reacted, degradation rate is 95.8%;The degradation rate of commodity nano titanium oxide P25 is 68.4% under the same conditions, and activity improves 40.1%.
Embodiment 3
Add 100g butyl titanates, 800g ethanol to stir in the reactor, control 40 DEG C of temperature, low whipping speed Under the conditions of 500-1000 rev/min, 10g polyacrylic acid is slowly added into, 1g polyvinylpyrrolidones, the mixed solution of 100g water, Four ester of metatitanic acid in system:Ethanol:Polyacrylic acid:Polyvinylpyrrolidone:Mass ratio=100 of water:800:10:1:100;Constant temperature Vitreosol is formed after stirring reaction 2h, 50g commodity nano titanium oxide P25 are added, starts ultrasonic agitation, continue 1h, shape Into translucent colloid;Pressure spray dryer device of the colloid for obtaining using routine, at pressure 10MPa, 150 DEG C of hot-air The nano titanium dioxide photocatalyst of double particle diameter distributions is obtained.As a result similar to Fig. 1, small particle average out to 6nm, big particle diameter are average For 26nm.
Application effect:Catalyst obtained in 1g is taken, plus 999g pure water stirring 0.5h can be prepared by the 0.1% of stable dispersion Nano titanium dioxide photocatalyst spray coating liquor, placement will not be layered for 8 months.The catalyst of preparation photocatalysis drop under sunlight Organic methyl orange in Xie Shui, under the conditions of catalyst amount 1g/L, methyl orange concentration 20mg/L, reacts 3h, and degradation rate is 95.6%;The degradation rate of commodity nano titanium oxide P25 is 54.2% under the same conditions, and activity improves 76.4%.
Embodiment 4
Add 100g butyl titanates, 300g ethanol to stir in the reactor, control temperature 60 C, low whipping speed Under the conditions of 500-1000 rev/min, 5g polyacrylic acid is slowly added into, 5g polyvinylpyrrolidones, the mixed solution of 1000g water, Four ester of metatitanic acid in system:Ethanol:Polyacrylic acid:Polyvinylpyrrolidone:Mass ratio=100 of water:300:5:5:1000;Constant temperature Vitreosol is formed after stirring reaction 4h, 100g commodity nano titanium oxide P25 are added, starts ultrasonic agitation, continue 3h, shape Into translucent colloid;Pressure spray dryer device of the colloid for obtaining using routine, at pressure 8MPa, 250 DEG C of hot-air The nano titanium dioxide photocatalyst of double particle diameter distributions is obtained.As a result similar to Fig. 2, Fig. 3, small particle average out to are shown in statistical result 10nm, big particle diameter average out to 30nm.
Application effect:Catalyst obtained in 5g is taken, plus 995g pure water stirring 0.5h can be prepared by the 0.5% of stable dispersion Nano titanium dioxide photocatalyst spray coating liquor, placement will not be layered for 6 months.The catalyst of preparation photocatalysis drop under sunlight Solution air Organic substance formaldehyde, in catalyst amount 0.1g/M3, concentration of formaldehyde 10mg/M3Under the conditions of, 2h is reacted, degradation rate is 97.6%;The degradation rate of commodity nano titanium oxide P25 is 68.4% under the same conditions, and activity improves 42.7%.
Embodiment 5
Add 100g tetraisopropyl titanates, 100g ethylene glycol to stir in the reactor, control temperature 50 C, in stirring Under the conditions of speed 500-1000 rev/min, 2g polyacrylic acid is slowly added into, 1g polyvinylpyrrolidones, the mixing of 800g water are molten Liquid, four ester of metatitanic acid in system:Ethanol:Polyacrylic acid:Polyvinylpyrrolidone:Mass ratio=100 of water:100:2:1:800;It is permanent Vitreosol is formed after warm stirring reaction 3h, 80g commodity nano titanium oxide P25 are added, starts ultrasonic agitation, continue 2h, Form translucent colloid;Pressure spray dryer device of the colloid for obtaining using routine, in pressure 5MPa, 250 DEG C of hot-air The lower nano titanium dioxide photocatalyst that double particle diameter distributions are obtained.As a result similar to Fig. 1, Fig. 4 is shown in statistical result, and little particle is average Particle diameter is 5nm, and bulky grain mean diameter is 25nm.
Application effect:Catalyst obtained in 20g is taken, plus 980g pure water stirring 0.5h can be prepared by the 2% of stable dispersion Nano titanium dioxide photocatalyst spray coating liquor, placement will not be layered for 6 months.The catalyst of preparation photocatalysis drop under sunlight Organic methyl orange in Xie Shui, under the conditions of catalyst concn 1g/L, methyl orange concentration 20mg/L, reacts 3h, and degradation rate is 86.7%;The degradation rate of commodity nano titanium oxide P25 is 54.2% under the same conditions, and activity improves 60.0%.

Claims (4)

1. nano titanium dioxide photocatalyst of a kind of pair of particle diameter distribution and preparation method thereof, it is characterised in that including following step Suddenly:
(1) organic titanate of certain mass is dissolved in alcoholic solution, unlatching is stirred and is slowly added into a certain amount of polypropylene Acid and the aqueous solution of polyvinylpyrrolidone, be hydrolyzed at 30~60 DEG C 2~6h of reaction, obtains transparent titanium dioxide molten Glue;
(2) given commodity nano titanium dioxide powder is added to into (1) described colloidal sol, 0.5~3h of ultrasonic agitation is obtained It is bright to translucent colloidal tio 2;
(3) complex that (2) obtain is spray-dried, the nano titanium dioxide photocatalyst of double particle diameter distributions is obtained.
2. method according to claim 1, it is characterised in that in step (1), organic titanate:Alcohol:Polyacrylic acid:It is poly- Vinylpyrrolidone:The mass ratio of water is:100:100~800:1~10:0.1~5:100~1000.Wherein, organic titanate For butyl titanate or tetraisopropyl titanate;Alcohol is ethanol, propanol, ethylene glycol.
3. method according to claim 1, it is characterised in that in step (2), commodity nano titanium oxide addition with have The mass ratio of machine titanate is 10~100:100;Preferred commodity nano titanium oxide is market plain edition P25 nanometer titanium dioxide Titanium.
4. method according to claim 1, it is characterised in that in step (3), is spray-dried using conventional press atomization Drying device, pressure 1-10Mpa;Hot-air is dried medium, temperature 150-250 DEG C.
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CN109023918A (en) * 2018-07-11 2018-12-18 澳洋集团有限公司 A kind of preparation method of uvioresistant cotton fabric
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CN107570132A (en) * 2017-08-28 2018-01-12 广州市华之特奥因特种材料科技有限公司 It can be seen that the preparation method of light photocatalyst
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CN109023918A (en) * 2018-07-11 2018-12-18 澳洋集团有限公司 A kind of preparation method of uvioresistant cotton fabric
CN114618528A (en) * 2022-04-02 2022-06-14 吉林化工学院 Ti having photocatalytic propertiesO2/CuInS2Preparation method and application of hollow nanospheres

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