CN108906016A - A kind of preparation method of porous titanium dioxide photocatalysis material - Google Patents

A kind of preparation method of porous titanium dioxide photocatalysis material Download PDF

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CN108906016A
CN108906016A CN201810681421.3A CN201810681421A CN108906016A CN 108906016 A CN108906016 A CN 108906016A CN 201810681421 A CN201810681421 A CN 201810681421A CN 108906016 A CN108906016 A CN 108906016A
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titanium dioxide
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weight
carbon fiber
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高坤
张瑞锋
刘伟
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Jiangsu Environmental Protection Science And Technology Co Ltd
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    • 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
    • B01J21/18Carbon
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    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/60Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
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    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02Impregnation, coating or precipitation
    • B01J37/0201Impregnation
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Abstract

This application discloses a kind of preparation methods of porous titanium dioxide photocatalysis material, including:(1), the lauryl amine of 3~7 parts by weight is added in absolute ethanol solution, is configured to the solution of 3.5~6mmol/L, the butyl carbonate of 1.2~2 parts by weight is then added, is stirred 10~60min.It is heated 10~36 hours under the conditions of 100~120 DEG C, reaction product centrifugation obtains solid product, then clean repeatedly to solid product using the mixed solution of ethyl alcohol and nitric acid, obtains poriferous titanium dioxide after dry;(2), compound concentration is in 5~7% titanium deoxide catalyst suspension;(3), hollow carbon fiber carrier is prepared;(4), by hollow carbon fiber carrier impregnation, 20~60min, lifting are dry after coming out in titanium dioxide composite photocatalyst suspension;By hollow carbon fiber carrier impregnation, 10~60min, lifting are dry after coming out in titanium dioxide optical catalyst suspension.Its Formaldehyde decomposition speed of material of the invention is fast, and degradation rate is high, and formaldehyde gas degradation rate can reach 93%, and degradation of toluene rate reaches 69.7%.

Description

A kind of preparation method of porous titanium dioxide photocatalysis material
Technical field
This application involves technical field of air purification, more particularly to a kind of preparation of porous titanium dioxide photocatalysis material Method.
Background technique
Studies have shown that photocatalysis technology has good application prospect photochemical catalyst that can divide in terms of environmental pollution improvement It dissipates and light catalyzed coating is made in resin, can not only make coating that there is excellent performance, can also be effectively reduced in environment dirty The concentration of metachromia gas makes organic or inorganic pollutant that redox reaction occur under photocatalysis, generates H2O、CO2And The substances such as salt reach innoxious, thus environment purification.
Titanium dioxide (TiO2), photon can be captured and realize separation of charge, be most common catalysis material.Such nothing The photocatalytic process of machine semiconductor light-catalyst be by light excitation generate electrons and holes, respectively be adsorbed onto catalyst The species on surface occur reduction and oxidation reaction and realize.But its photochemical catalyst powder faces photocatalysis in application process The problems such as low efficiency and low adsorbance.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of porous titanium dioxide photocatalysis material, to overcome existing skill Deficiency in art.
To achieve the above object, the present invention provides the following technical solutions:
The embodiment of the present application discloses a kind of preparation method of porous titanium dioxide photocatalysis material, including:
(1), the lauryl amine of 3~7 parts by weight is added in absolute ethanol solution, is configured to the molten of 3.5~6mmol/L Then liquid is added the butyl carbonate of 1.2~2 parts by weight, is stirred 10~60min.10 are heated under the conditions of 100~120 DEG C ~36 hours, reaction product centrifugation obtained solid product, was then carried out using the mixed solution of ethyl alcohol and nitric acid to solid product Cleaning repeatedly, obtains poriferous titanium dioxide after dry;
(2), poriferous titanium dioxide is added into deionized water, it is outstanding in 5~7% titanium deoxide catalysts is configured to concentration Supernatant liquid;
(3), hollow carbon fiber carrier is prepared;
(4), 20~60min, lifting in titanium dioxide composite photocatalyst suspension by hollow carbon fiber carrier impregnation In 90~120 DEG C of dry 60~120min after out;Continue the hollow carbon fiber carrier impregnation after drying in titanium-dioxide photo 10~60min in catalyst suspension obtains poriferous titanium dioxide light in 60~120 DEG C of dry 30~90min after lifting out Catalysis material.
Preferably, in the preparation method of above-mentioned porous titanium dioxide photocatalysis material, step (2) includes:In room temperature Under the conditions of, sodium hydrogen telluride, poriferous titanium dioxide are add to deionized water, 10~30min of magnetic agitation;Then acetic acid is added Cadmium, mercaptopropionic acid 10~30min of ultrasonic disperse obtain titanium deoxide catalyst suspension.
Preferably, in the preparation method of above-mentioned porous titanium dioxide photocatalysis material, the sodium hydrogen telluride and porous The weight ratio of titanium dioxide is (30~50):(150~200).
Preferably, in the preparation method of above-mentioned porous titanium dioxide photocatalysis material, the cadmium acetate and sulfydryl third The weight ratio of acid is (60~80):(50~60).
Preferably, in the preparation method of above-mentioned porous titanium dioxide photocatalysis material, titanium deoxide catalyst suspends Liquid mass concentration is 6.4%.
Preferably, in the preparation method of above-mentioned porous titanium dioxide photocatalysis material, step (3) includes:
Under 370~450 DEG C of hot conditions, spinning is carried out to polyacrylonitrile by spinning machine, obtains doughnut, then In chemical crosslinking device, oxygen, which is added, makes it react 20~30min at 50~60 DEG C, washs to doughnut, removes Then the impurity on surface first impregnates 8~15min in an acidic solution, wash to neutrality, then proceed to impregnate in alkaline solution 10~20min is washed to neutrality, is then carbonized 1~3 hour in 2500~2800 DEG C of graphitizing furnace.
Disclosed herein as well is a kind of preparation methods of porous titanium dioxide photocatalysis material, including:
(1), the lauryl amine of 3 parts by weight is added in absolute ethanol solution, is configured to the solution of 4mmol/L, then plus The butyl carbonate for entering 1.5 parts by weight, is stirred 20min, heats 16 hours under the conditions of 100 DEG C, and reaction product centrifugation obtains Then solid product clean repeatedly, obtains porous two after dry using the mixed solution of ethyl alcohol and nitric acid to solid product Titanium oxide;
(2), under normal temperature conditions, the poriferous titanium dioxide of the sodium hydrogen telluride of 45 parts by weight, 180 parts by weight is added to In ionized water, magnetic agitation 20min;Then the cadmium acetate of 70 parts by weight, the mercaptopropionic acid ultrasonic disperse of 55 parts by weight is added 10min obtains mass concentration in 6.4% titanium dioxide composite photocatalyst suspension;
(3), under 400 DEG C of hot conditions, spinning is carried out to polyacrylonitrile by spinning machine, obtains doughnut, then In chemical crosslinking device, oxygen, which is added, makes it react 30min at 60 DEG C, washs to doughnut, removes the miscellaneous of surface Then matter first impregnates 10min in an acidic solution, washing to neutrality then proceedes to impregnate 10min in alkaline solution, washs It to neutrality, is then carbonized 2 hours in 2600 DEG C of graphitizing furnace, obtains hollow carbon fiber carrier;
(4), by hollow carbon fiber carrier impregnation, 40min, lifting are come out in titanium dioxide composite photocatalyst suspension Afterwards in 110 DEG C of dry 120min;Continue the hollow carbon fiber carrier impregnation after drying to hang in titanium dioxide composite photocatalyst 10min in supernatant liquid obtains composite photocatalyst material in 110 DEG C of dry 70min after lifting out.
Compared with the prior art, the advantages of the present invention are as follows:Its Formaldehyde decomposition speed of material of the invention is fast, and degradation rate Height, formaldehyde gas degradation rate can reach 93%, and degradation of toluene rate reaches 69.7%.
Specific embodiment
The present invention is described further by the following example:According to following embodiments, the present invention may be better understood. However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
Embodiment 1
The lauryl amine of 3 parts by weight is added in absolute ethanol solution, the solution of 4mmol/L is configured to, is then added 1.5 The butyl carbonate of parts by weight, is stirred 20min.It is heated 16 hours under the conditions of 100 DEG C, reaction product centrifugation obtains solid and produces Then object clean repeatedly, obtains poriferous titanium dioxide after dry using the mixed solution of ethyl alcohol and nitric acid to solid product.
Under normal temperature conditions, the poriferous titanium dioxide of the sodium hydrogen telluride of 45mg, 180mg are add to deionized water, magnetic Power stirs 20min;Then the cadmium acetate of 70mg, the mercaptopropionic acid ultrasonic disperse 10min of 55mg is added, obtains mass concentration and exists 6.4% titanium dioxide composite photocatalyst suspension.
Under 400 DEG C of hot conditions, spinning is carried out to polyacrylonitrile by spinning machine, doughnut is obtained, is then changing It learns in crosslinking device, oxygen, which is added, makes it react 30min at 60 DEG C.Doughnut is washed, removes the impurity on surface, so First impregnate 10min in an acidic solution afterwards, washing to neutrality then proceedes to impregnate 10min in alkaline solution, washs into Property, it is then carbonized 2 hours in 2600 DEG C of graphitizing furnace, obtains hollow carbon fiber carrier.
By hollow carbon fiber carrier impregnation in titanium dioxide composite photocatalyst suspension 40min, lifting come out after 110 DEG C of dry 120min;Continue the hollow carbon fiber carrier impregnation after drying in titanium dioxide composite photocatalyst suspension Middle 10min obtains composite photocatalyst material in 110 DEG C of dry 70min after lifting out.
Degradation test is carried out in closed space PARA FORMALDEHYDE PRILLS(91,95) and toluene, controls 22 DEG C of environment temperature, gas flow rate 1.5m/s, Envionmental humidity is 45%, initial concentration of formaldehyde 5mg/m3, the initial concentration of toluene is 0.7mg/m3, it can be found that:
Concentration of formaldehyde is stablized after 50min, and formaldehyde gas degradation rate reaches 96.1%, and after 70min, toluene concentration reaches Stablize, degradation of toluene rate reaches 84%.
Comparative example 1
Under normal temperature conditions, the titanium dioxide of 200mg is add to deionized water, magnetic agitation 20min;Obtain quality Concentration is in 6% titanium dioxide optical catalyst suspension.
Under 400 DEG C of hot conditions, spinning is carried out to polyacrylonitrile by spinning machine, doughnut is obtained, is then changing It learns in crosslinking device, oxygen, which is added, makes it react 30min at 60 DEG C.Doughnut is washed, removes the impurity on surface, so First impregnate 10min in an acidic solution afterwards, washing to neutrality then proceedes to impregnate 10min in alkaline solution, washs into Property, it is then carbonized 2 hours in 2600 DEG C of graphitizing furnace, obtains hollow carbon fiber carrier.
The aluminium hydroxide of 40mg is added into the orthophosphoric acid of 100mL, ortho-phosphoric mass fraction is 85%, is heated to 70 DEG C~85 DEG C, binder is obtained after being stirred 20min.
By hollow carbon fiber carrier impregnation 5min in a binder, in 90~100 DEG C of dryings after then lifting comes out 10min;Continue the 40min in titanium dioxide optical catalyst suspension of the hollow carbon fiber carrier impregnation after drying, lifts out In 110 DEG C of dry 120min after coming;Continue the hollow carbon fiber carrier impregnation after drying in titanium dioxide composite photocatalyst 10min in suspension obtains composite photocatalyst material in 110 DEG C of dry 70min after lifting out.
Degradation test is carried out in closed space PARA FORMALDEHYDE PRILLS(91,95) and toluene, controls 22 DEG C of environment temperature, gas flow rate 1.5m/s, Envionmental humidity is 45%, initial concentration of formaldehyde 5mg/m3, the initial concentration of toluene is 0.7mg/m3, it can be found that:
Concentration of formaldehyde is stablized after 100min, and formaldehyde gas degradation rate reaches 84.7%.After 120min, toluene concentration reaches To stabilization, degradation of toluene rate reaches 69.7%.
Comparative example 2
Under normal temperature conditions, the titanium dioxide of the sodium hydrogen telluride of 40mg, 200mg are add to deionized water, magnetic force stirs Mix 20min;Then the cadmium acetate of 80mg, the mercaptopropionic acid ultrasonic disperse 10min of 50mg is added, obtains mass concentration 6% 2 Titanium oxide composite photo-catalyst suspension.
Commercially available carbon fiber is provided as carrier (STF-1000T type, Jiangsu Sutong Carbon Fiber Co., Ltd).
The aluminium hydroxide of 40mg is added into the orthophosphoric acid of 100mL, ortho-phosphoric mass fraction is 85%, is heated to 70 DEG C~85 DEG C, binder is obtained after being stirred 20min.
By carrier impregnation 5min in a binder, in 90~100 DEG C of dry 10min after then lifting comes out;Continue to do Carrier impregnation after the dry 40min in titanium dioxide composite photocatalyst suspension, lifting come out after in 110 DEG C of dryings 120min;Continue the carrier impregnation after drying the 10min in titanium dioxide composite photocatalyst suspension, lifting come out after 110 DEG C of dry 70min obtain composite photocatalyst material.
Degradation test is carried out in closed space PARA FORMALDEHYDE PRILLS(91,95) and toluene, controls 22 DEG C of environment temperature, gas flow rate 1.5m/s, Envionmental humidity is 45%, initial concentration of formaldehyde 5mg/m3, the initial concentration of toluene is 0.7mg/m3, it can be found that:
Concentration of formaldehyde is stablized after 90min, and formaldehyde gas degradation rate reaches 86.2%.After 120min, toluene concentration reaches To stabilization, degradation of toluene rate reaches 73.4%.
It is compared with comparative example 1-2 it is found that the Degradation Formaldehyde effect and degradation of toluene rate of embodiment 1 are obviously high by embodiment 1 In documents 1 and documents 2.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive Property include so that include a series of elements process, method, article or equipment not only include those elements, but also Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic Element.

Claims (7)

1. a kind of preparation method of porous titanium dioxide photocatalysis material, which is characterized in that including:
(1), the lauryl amine of 3~7 parts by weight is added in absolute ethanol solution, is configured to the solution of 3.5~6mmol/L, so The butyl carbonate of 1.2~2 parts by weight is added afterwards, is stirred 10~60min.Heating 10~36 is small under the conditions of 100~120 DEG C When, reaction product centrifugation obtains solid product, is then cleaned using the mixed solution of ethyl alcohol and nitric acid to solid product more It is secondary, poriferous titanium dioxide is obtained after dry;
(2), poriferous titanium dioxide is added into deionized water, is configured to concentration and suspends in 5~7% titanium deoxide catalysts Liquid;
(3), hollow carbon fiber carrier is prepared;
(4), by hollow carbon fiber carrier impregnation, 20~60min, lifting are come out in titanium dioxide composite photocatalyst suspension Afterwards in 90~120 DEG C of dry 60~120min;Continue the hollow carbon fiber carrier impregnation after drying in optically catalytic TiO 2 10~60min in agent suspension obtains porous titanium dioxide photocatalysis in 60~120 DEG C of dry 30~90min after lifting out Material.
2. the preparation method of porous titanium dioxide photocatalysis material according to claim 1, which is characterized in that step (2) Including:Under normal temperature conditions, sodium hydrogen telluride, poriferous titanium dioxide are add to deionized water, 10~30min of magnetic agitation; Then cadmium acetate, mercaptopropionic acid 10~30min of ultrasonic disperse is added, obtains titanium deoxide catalyst suspension.
3. the preparation method of porous titanium dioxide photocatalysis material according to claim 2, which is characterized in that the tellurium hydrogen The weight ratio for changing sodium and poriferous titanium dioxide is (30~50):(150~200).
4. the preparation method of porous titanium dioxide photocatalysis material according to claim 2, which is characterized in that the acetic acid The weight ratio of cadmium and mercaptopropionic acid is (60~80):(50~60).
5. the preparation method of porous titanium dioxide photocatalysis material according to claim 1, which is characterized in that titanium dioxide Catalyst suspension mass concentration is 6.4%.
6. the preparation method of porous titanium dioxide photocatalysis material according to claim 1, which is characterized in that step (3) Including:
Under 370~450 DEG C of hot conditions, spinning is carried out to polyacrylonitrile by spinning machine, doughnut is obtained, is then changing It learns in crosslinking device, oxygen, which is added, makes it react 20~30min at 50~60 DEG C, washs to doughnut, removes surface Impurity, then first impregnate 8~15min in an acidic solution, washing to neutrality, then proceed to impregnate 10 in alkaline solution~ 20min is washed to neutrality, is then carbonized 1~3 hour in 2500~2800 DEG C of graphitizing furnace.
7. a kind of preparation method of porous titanium dioxide photocatalysis material, which is characterized in that including:
(1), the lauryl amine of 3 parts by weight is added in absolute ethanol solution, is configured to the solution of 4mmol/L, is then added 1.5 The butyl carbonate of parts by weight, is stirred 20min, heats 16 hours under the conditions of 100 DEG C, and reaction product centrifugation obtains solid and produces Then object clean repeatedly, obtains poriferous titanium dioxide after dry using the mixed solution of ethyl alcohol and nitric acid to solid product;
(2), the poriferous titanium dioxide of the sodium hydrogen telluride of 45 parts by weight, 180 parts by weight under normal temperature conditions, is added to deionization In water, magnetic agitation 20min;Then the cadmium acetate of 70 parts by weight, the mercaptopropionic acid ultrasonic disperse 10min of 55 parts by weight is added, Mass concentration is obtained in 6.4% titanium dioxide composite photocatalyst suspension;
(3), under 400 DEG C of hot conditions, spinning is carried out to polyacrylonitrile by spinning machine, doughnut is obtained, is then changing It learns in crosslinking device, oxygen, which is added, makes it react 30min at 60 DEG C, washs to doughnut, removes the impurity on surface, so First impregnate 10min in an acidic solution afterwards, washing to neutrality then proceedes to impregnate 10min in alkaline solution, washs into Property, it is then carbonized 2 hours in 2600 DEG C of graphitizing furnace, obtains hollow carbon fiber carrier;
(4), by hollow carbon fiber carrier impregnation in titanium dioxide composite photocatalyst suspension 40min, lifting come out after 110 DEG C of dry 120min;Continue the hollow carbon fiber carrier impregnation after drying in titanium dioxide composite photocatalyst suspension Middle 10min obtains composite photocatalyst material in 110 DEG C of dry 70min after lifting out.
CN201810681421.3A 2018-06-27 2018-06-27 A kind of preparation method of porous titanium dioxide photocatalysis material Withdrawn CN108906016A (en)

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CN115888817A (en) * 2022-11-03 2023-04-04 山东欧蓝素汽车环保科技有限公司 Preparation method of catkin-polydopamine-titanium dioxide porous photocatalyst

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CN108067267A (en) * 2017-12-19 2018-05-25 中国计量大学 A kind of visible light-responded cadmium telluride/titanium dioxide Z-type photochemical catalyst and its preparation method and application
CN108201789A (en) * 2017-12-19 2018-06-26 如皋六维环境科技有限公司 A kind of preparation method of purifying formaldehyde material and application

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Publication number Priority date Publication date Assignee Title
CN1594102A (en) * 2004-07-05 2005-03-16 华东理工大学 Method for preparing titanium dioxide mesoporous material
CN101513617A (en) * 2009-01-05 2009-08-26 浙江理工大学 Method for preparing carbon fiber loaded composite photocatalysis membrane
CN102786088A (en) * 2012-09-05 2012-11-21 中国工程物理研究院核物理与化学研究所 Preparation method of nano titanium dioxide compound
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115888817A (en) * 2022-11-03 2023-04-04 山东欧蓝素汽车环保科技有限公司 Preparation method of catkin-polydopamine-titanium dioxide porous photocatalyst
CN115888817B (en) * 2022-11-03 2024-04-30 山东欧蓝素汽车环保科技有限公司 Preparation method of flyy-poly-dopamine-titanium dioxide porous photocatalyst

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