CN109647370A - A kind of porous material and preparation method using sol-gal process carried titanium dioxide - Google Patents

A kind of porous material and preparation method using sol-gal process carried titanium dioxide Download PDF

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Publication number
CN109647370A
CN109647370A CN201910118876.9A CN201910118876A CN109647370A CN 109647370 A CN109647370 A CN 109647370A CN 201910118876 A CN201910118876 A CN 201910118876A CN 109647370 A CN109647370 A CN 109647370A
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porous material
sol
titanium dioxide
process carried
preparation
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Inventor
邓国民
李树逊
李军代
施曙东
岳国柱
邱轶
仕佳
宋健
徐如波
姚凯
何毅威
张玮
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SHANGHAI PUDONG ROAD BRIDGE CONSTRUCTION CO Ltd
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SHANGHAI PUDONG ROAD BRIDGE CONSTRUCTION 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
    • B01J21/18Carbon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/92Chemical or biological purification of waste gases of engine exhaust gases
    • B01D53/94Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0211Compounds of Ti, Zr, Hf
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B01J20/08Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057Surface area, e.g. B.E.T specific surface area
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/3085Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
    • 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
    • B01J21/02Boron or aluminium; Oxides or hydroxides thereof
    • B01J21/04Alumina
    • 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

Abstract

The present invention relates to the porous material and preparation method using sol-gal process carried titanium dioxide, porous material forms 5 parts -20 parts of titanium dioxide, 80 parts -95 parts of porous material by following mass component;The porous material is one of active carbon or activated alumina.Specific preparation method includes the preparation method of the preparation method using the active carbon of sol-gal process carried titanium dioxide and the activated alumina using sol-gal process carried titanium dioxide.Not only itself microporous structure is abundant for porous material of the present invention, large specific surface area, enriched gas capacity is big, and porous material surface chemical functional group is abundant, including a variety of acid and basic functionalities, after sol-gal process carried titanium dioxide, the type of function and effect enhancing and purification gas that vehicle exhaust is catalytically decomposed is more.In addition, the preparation method of the material is simpler, convenient.

Description

A kind of porous material and preparation method using sol-gal process carried titanium dioxide
Technical field
It is especially a kind of for pavement of road field purification vehicle exhaust and using molten the present invention relates to field of material technology The porous material and preparation method thereof of sol-gel carried titanium dioxide.
Background technique
The domestic at present correlative study about pavement of road field purification vehicle exhaust and engineer application test examples, Asphalt or brushing and road barrier will be directly incorporated into the photocatalysis Decomposition material based on titanium dioxide, still There are the deficiencies of essence for this application mode, and if exhaust collection capacity is limited, road is as open system, vehicle exhaust flowing Extremely irregular with spreading, therefore, the probability that the simple titanium dioxide for spraying or applying is contacted with tail gas is minimum;While simple two The type of titanium oxide processing gas is relatively simple, and result of study shows: titanium dioxide, which degrades to the hydrocarbon in automobile, imitates Rate is higher, can be lower to nitrogen oxides treatment efficiency, and the vehicle exhaust type being capable of handling is more single.
Therefore, it is necessary to study and develop it is a kind of for road field and collect capacity is big, treatment effeciency is high, large area with The convenient and fast purifying vehicle exhaust technology of large-scale application.
Summary of the invention
The purpose of the present invention is a kind of using the porous of sol-gal process carried titanium dioxide to solve the above problem Material and preparation method, not only itself microporous structure is abundant for the porous material, large specific surface area, and enriched gas capacity is big, and And porous material surface chemical functional group is abundant, including a variety of acid and basic functionalities, loads dioxy through sol-gal process After changing titanium, the type of function and effect enhancing and purification gas that vehicle exhaust is catalytically decomposed is more.In addition, the preparation side of the material Method is simpler, convenient.
Technical solution provided by the invention is as follows:
A kind of porous material using sol-gal process carried titanium dioxide is formed by following mass component:
5 parts -20 parts of titanium dioxide, 80 parts -95 parts of porous material;
The porous material is one of active carbon or activated alumina.
Preferably, the active carbon specific surface area is between 700m2/g-1500m2/g;
The activated alumina specific surface area is between 250m2/g-500m2/g.
The invention of this hair also provides a kind of preparation method of porous material using sol-gal process carried titanium dioxide, including Following preparation step:
S1, the porous material for weighing certain mass, the porous material are porous material described in any one of claim 1-2 Material, and the porous material is the active carbon, is washed with distilled water 3 times -10 times, 100 DEG C of constant temperature dehydrations in vacuum oven >=12h, it is spare;
S2,24mL dehydrated alcohol is taken, instills a small amount of nitric acid;
S3,6mL tetra-n-butyl titanate is measured, stirs lower instill in ethanol solution prepared in S2;
The spare active carbon that S4, the S1 for weighing 10g-100G are prepared, is added in S3, is vigorously stirred with magnetic stirring apparatus 20min-60min;
S5,5mL distilled water and 13mL dehydrated alcohol are measured respectively, are made into mixed solution, control rate of titration 30d/min, It slowly instills in S4 reaction system under constant stirring;
S6, continue to stir 10min, stand, obtain black sol;
S7, obtained gel is put into 60 DEG C of thermostatic drying chamber >=12h, so that the dehydrated alcohol in colloid is slowly volatilized dry Only;
It is ground after S8, drying with mortar, is packed into crucible, is put into the Muffle furnace of nitrogen protection, muffle furnace rises to pre- If keeping the temperature calcination time when temperature, room temperature cooling later obtains the porous material using sol-gal process carried titanium dioxide.
Preferably, in step S2, the analysis of the dehydrated alcohol is pure 95% or so, and makes it after instilling a small amount of nitric acid PH value is 3.5.
Preferably, in step S3, the SILVER REAGENT of the tetra-n-butyl titanate is 99% or so.
Preferably, in step S5, the analysis of the dehydrated alcohol is pure 95% or so.
Preferably, in step S8, the preset temperature is at 450 DEG C or so, and Muffle furnace heating rate is 5 DEG C/min left The right side, heat preservation calcination time are 4h.
The present invention also provides a kind of preparation methods of porous material using sol-gal process carried titanium dioxide, including with Lower preparation step:
S01,6mL tetra-n-butyl titanate is measured, stirred in AR grades of ethanol solutions of lower instillation, addition inhibits while stirring Agent glacial acetic acid, until butyl titanate forms the colloidal solution of chelate;
S02, deionized water is added in the colloidal solution of preparation, colloidal particle is made to form a kind of skeleton structure of opening, It is slowly added to porous material simultaneously, the porous material is porous material described in any one of claim 1-2, and described porous Material is the activated alumina, until colloidal solution loses flowability, forms gel;
S03, at 100 DEG C by gel freeze-day with constant temperature >=for 24 hours, remove moisture, organic group and organic solvent in gel;
It is ground after S04, drying with mortar, is packed into crucible, is put into the Muffle furnace of nitrogen protection, muffle furnace rises to pre- If keeping the temperature calcination time when temperature, room temperature cooling later obtains the porous material using sol-gal process carried titanium dioxide.
Preferably, in step S04, the preset temperature is at 450 DEG C or so, and Muffle furnace heating rate is 5 DEG C/min left The right side, heat preservation calcination time are 4h.
In conclusion a kind of porous material and preparation side using sol-gal process carried titanium dioxide provided by the invention Having the characteristics that for method is following:
1, there is gas enrichment function
Only having the function of purification gas compared with prior art, porous material of the present invention not only has gas purifying function, and And tail gas can be effectively enriched with by its micropore and bigger serface abundant, prevent tail gas from entering atmospheric environment to greatest extent.
2, the type of purification gas is more
It is catalyzed compared to ordinary titanium dioxide, porous material of the present invention, either active carbon or activated alumina, inside Active higher chemical functional group can not only further enhance titanium dioxide degradable vehicle exhaust under light environment Ability, and can also induce and expand the type of purification vehicle exhaust.
3, preparation method simplicity is convenient
Present invention sol-gal process is convenient in the simple process of porous material by titanium dichloride load.
Specific embodiment
The present invention provides a kind of porous material using sol-gal process carried titanium dioxide, is specifically shown in following embodiment:
Embodiment one:
5 parts of titanium dioxide, 95 parts of porous material;And porous material is one of active carbon or activated alumina.Such as: more Porous materials are active carbon specific surface area in 700m2/g-1500m2/g;Porous material is activated alumina specific surface area in 250m2/ g-500m2/g。
Embodiment two:
20 parts of titanium dioxide, 80 parts of porous material;And porous material is one of active carbon or activated alumina.Such as: Porous material is active carbon specific surface area in 700m2/g-1500m2/g;Porous material is that activated alumina specific surface area exists 250m2/g-500m2/g。
The invention of this hair also provides a kind of reality of the preparation method of porous material using sol-gal process carried titanium dioxide Example is applied, the preparation method of the active carbon of sol-gal process carried titanium dioxide, including following preparation step are mainly used:
Embodiment one:
S1, the porous material for weighing certain mass are active carbon, are washed with distilled water 3 times -10 times, in vacuum oven 100 DEG C of constant temperature dehydration >=12h, it is spare;
S2,24mL dehydrated alcohol is taken, instills a small amount of nitric acid;
S3,6mL tetra-n-butyl titanate is measured, stirs lower instill in ethanol solution prepared in S2;
The spare active carbon that S4, the S1 for weighing 10g-100G are prepared, is added in S3, is vigorously stirred with magnetic stirring apparatus 20min-60min;
S5,5mL distilled water and 13mL dehydrated alcohol are measured respectively, are made into mixed solution, control rate of titration 30d/min, It slowly instills in S4 reaction system under constant stirring;
S6, continue to stir 10min, stand, obtain black sol;
S7, obtained gel is put into 60 DEG C of thermostatic drying chamber >=12h, so that the dehydrated alcohol in colloid is slowly volatilized dry Only;
It is ground after S8, drying with mortar, is packed into crucible, is put into the Muffle furnace of nitrogen protection, muffle furnace rises to pre- If keeping the temperature calcination time when temperature, room temperature cooling later obtains the porous material using sol-gal process carried titanium dioxide.
Embodiment two:
S1, the porous material for weighing certain mass, porous material are active carbon, are washed with distilled water 3 times -10 times, vacuum 100 DEG C of constant temperature dehydration >=12h, spare in drying box;
S2,24mL dehydrated alcohol is taken, instills a small amount of nitric acid, wherein the analysis of dehydrated alcohol is pure 95% or so, and drips Make its pH value 3.5 after entering a small amount of nitric acid;
S3,6mL tetra-n-butyl titanate is measured, stirs lower instill in ethanol solution prepared in S2;
The spare active carbon that S4, the S1 for weighing 10g-100G are prepared, is added in S3, is vigorously stirred with magnetic stirring apparatus 20min-60min;
S5,5mL distilled water and 13mL dehydrated alcohol are measured respectively, are made into mixed solution, control rate of titration 30d/min, It slowly instills in S4 reaction system under constant stirring;
S6, continue to stir 10min, stand, obtain black sol;
S7, obtained gel is put into 60 DEG C of thermostatic drying chamber >=12h, so that the dehydrated alcohol in colloid is slowly volatilized dry Only;
It is ground after S8, drying with mortar, is packed into crucible, is put into the Muffle furnace of nitrogen protection, muffle furnace rises to pre- If keeping the temperature calcination time when temperature, room temperature cooling later obtains the porous material using sol-gal process carried titanium dioxide.
Embodiment three:
S1, the porous material for weighing certain mass, porous material are active carbon, are washed with distilled water 3 times -10 times, vacuum 100 DEG C of constant temperature dehydration >=12h, spare in drying box;
S2,24mL dehydrated alcohol is taken, instills a small amount of nitric acid;
S3,6mL tetra-n-butyl titanate is measured, the SILVER REAGENT of tetra-n-butyl titanate stirs lower instill in S2 99% or so In prepared ethanol solution;
The spare active carbon that S4, the S1 for weighing 10g-100G are prepared, is added in S3, is vigorously stirred with magnetic stirring apparatus 20min-60min;
S5,5mL distilled water and 13mL dehydrated alcohol are measured respectively, are made into mixed solution, control rate of titration 30d/min, It slowly instills in S4 reaction system under constant stirring;
S6, continue to stir 10min, stand, obtain black sol;
S7, obtained gel is put into 60 DEG C of thermostatic drying chamber >=12h, so that the dehydrated alcohol in colloid is slowly volatilized dry Only;
It is ground after S8, drying with mortar, is packed into crucible, is put into the Muffle furnace of nitrogen protection, muffle furnace rises to pre- If keeping the temperature calcination time when temperature, room temperature cooling later obtains the porous material using sol-gal process carried titanium dioxide.
Example IV:
S1, the porous material for weighing certain mass, porous material are active carbon, are washed with distilled water 3 times -10 times, vacuum 100 DEG C of constant temperature dehydration >=12h, spare in drying box;
S2,24mL dehydrated alcohol is taken, instills a small amount of nitric acid;
S3,6mL tetra-n-butyl titanate is measured, stirs lower instill in ethanol solution prepared in S2;
The spare active carbon that S4, the S1 for weighing 10g-100G are prepared, is added in S3, is vigorously stirred with magnetic stirring apparatus 20min-60min;
S5,5mL distilled water and 13mL dehydrated alcohol are measured respectively, wherein the analysis of dehydrated alcohol is pure 95% or so, matches At mixed solution, rate of titration 30d/min is controlled, is slowly instilled in S4 reaction system under constant stirring;
S6, continue to stir 10min, stand, obtain black sol;
S7, obtained gel is put into 60 DEG C of thermostatic drying chamber >=12h, so that the dehydrated alcohol in colloid is slowly volatilized dry Only;
It is ground after S8, drying with mortar, is packed into crucible, is put into the Muffle furnace of nitrogen protection, muffle furnace rises to pre- If keeping the temperature calcination time when temperature, room temperature cooling later obtains the porous material using sol-gal process carried titanium dioxide.
Embodiment five:
S1, the porous material for weighing certain mass, porous material are active carbon, are washed with distilled water 3 times -10 times, vacuum 100 DEG C of constant temperature dehydration >=12h, spare in drying box;
S2,24mL dehydrated alcohol is taken, instills a small amount of nitric acid;
S3,6mL tetra-n-butyl titanate is measured, stirs lower instill in ethanol solution prepared in S2;
The spare active carbon that S4, the S1 for weighing 10g-100G are prepared, is added in S3, is vigorously stirred with magnetic stirring apparatus 20min-60min;
S5,5mL distilled water and 13mL dehydrated alcohol are measured respectively, are made into mixed solution, control rate of titration 30d/min, It slowly instills in S4 reaction system under constant stirring;
S6, continue to stir 10min, stand, obtain black sol;
S7, obtained gel is put into 60 DEG C of thermostatic drying chamber >=12h, so that the dehydrated alcohol in colloid is slowly volatilized dry Only;
It is ground after S8, drying with mortar, is packed into crucible, is put into the Muffle furnace of nitrogen protection, muffle furnace rises to pre- If keeping the temperature calcination time when temperature, room temperature cooling later obtains the porous material using sol-gal process carried titanium dioxide. Wherein, preset temperature is at 450 DEG C or so, and Muffle furnace heating rate is 5 DEG C/min or so, and heat preservation calcination time is 4h.
The invention of this hair also provides a kind of reality of the preparation method of porous material using sol-gal process carried titanium dioxide Example is applied, the preparation method of the activated alumina of sol-gal process carried titanium dioxide, including following preparation step are mainly used It is rapid:
Embodiment one:
S01,6mL tetra-n-butyl titanate is measured, stirred in AR grades of ethanol solutions of lower instillation, addition inhibits while stirring Agent glacial acetic acid, until butyl titanate forms the colloidal solution of chelate;
S02, deionized water is added in the colloidal solution of preparation, colloidal particle is made to form a kind of skeleton structure of opening, It is slowly added to porous material simultaneously, porous material is activated alumina, until colloidal solution loses flowability, forms gel;
S03, at 100 DEG C by gel freeze-day with constant temperature >=for 24 hours, remove moisture, organic group and organic solvent in gel;
It is ground after S04, drying with mortar, is packed into crucible, is put into the Muffle furnace of nitrogen protection, muffle furnace rises to pre- If keeping the temperature calcination time when temperature, room temperature cooling later obtains the porous material using sol-gal process carried titanium dioxide.
Embodiment two:
S01,6mL tetra-n-butyl titanate is measured, stirred in AR grades of ethanol solutions of lower instillation, addition inhibits while stirring Agent glacial acetic acid, until butyl titanate forms the colloidal solution of chelate;
S02, deionized water is added in the colloidal solution of preparation, colloidal particle is made to form a kind of skeleton structure of opening, It is slowly added to porous material simultaneously, porous material is activated alumina, until colloidal solution loses flowability, forms gel;
S03, at 100 DEG C by gel freeze-day with constant temperature >=for 24 hours, remove moisture, organic group and organic solvent in gel;
It is ground after S04, drying with mortar, is packed into crucible, is put into the Muffle furnace of nitrogen protection, muffle furnace rises to pre- If keeping the temperature calcination time when temperature, room temperature cooling later obtains the porous material using sol-gal process carried titanium dioxide. Wherein, preset temperature is at 450 DEG C or so, and Muffle furnace heating rate is 5 DEG C/min or so, and heat preservation calcination time is 4h.
It should be noted that above-described embodiment can be freely combined as needed.The above is only of the invention preferred Embodiment, it is noted that for those skilled in the art, in the premise for not departing from the principle of the invention Under, several improvements and modifications can also be made, these modifications and embellishments should also be considered as the scope of protection of the present invention.

Claims (9)

1. a kind of porous material using sol-gal process carried titanium dioxide, which is characterized in that formed by following mass component:
5 parts -20 parts of titanium dioxide, 80 parts -95 parts of porous material;
The porous material is one of active carbon or activated alumina.
2. the porous material according to claim 1 using sol-gal process carried titanium dioxide, it is characterised in that:
The active carbon specific surface area is between 700m2/g-1500m2/g;
The activated alumina specific surface area is between 250m2/g-500m2/g.
3. a kind of preparation method of the porous material using sol-gal process carried titanium dioxide, which is characterized in that including following Preparation step:
S1, the porous material for weighing certain mass, the porous material are porous material described in any one of claim 1-2, And the porous material is the active carbon, is washed with distilled water 3 times -10 times, 100 DEG C of constant temperature dehydration in vacuum oven >= 12h, it is spare;
S2,24mL dehydrated alcohol is taken, instills a small amount of nitric acid;
S3,6mL tetra-n-butyl titanate is measured, stirs lower instill in ethanol solution prepared in S2;
The spare active carbon that S4, the S1 for weighing 10g-100G are prepared, is added in S3, is vigorously stirred with magnetic stirring apparatus 20min-60min;
S5,5mL distilled water and 13mL dehydrated alcohol are measured respectively, be made into mixed solution, rate of titration 30d/min is controlled, not It is slowly instilled in S4 reaction system under disconnected stirring;
S6, continue to stir 10min, stand, obtain black sol;
S7, obtained gel is put into 60 DEG C of thermostatic drying chamber >=12h, the dehydrated alcohol in colloid is made slowly to volatilize completely;
It is ground after S8, drying with mortar, is packed into crucible, be put into the Muffle furnace of nitrogen protection, muffle furnace rises to default temperature When spending, calcination time is kept the temperature, later the cooling porous material obtained using sol-gal process carried titanium dioxide of room temperature.
4. the preparation method of the porous material according to claim 3 using sol-gal process carried titanium dioxide, special Sign is:
In step S2, the analysis of the dehydrated alcohol is pure 95% or so, and makes its pH value 3.5 after instilling a small amount of nitric acid.
5. the preparation method of the porous material according to claim 3 using sol-gal process carried titanium dioxide, special Sign is:
In step S3, the SILVER REAGENT of the tetra-n-butyl titanate is 99% or so.
6. the preparation method of the porous material according to claim 3 using sol-gal process carried titanium dioxide, special Sign is:
In step S5, the analysis of the dehydrated alcohol is pure 95% or so.
7. the preparation method of the porous material according to claim 3 using sol-gal process carried titanium dioxide, special Sign is:
In step S8, the preset temperature is at 450 DEG C or so, and Muffle furnace heating rate is 5 DEG C/min or so, when heat preservation is calcined Between be 4h.
8. a kind of preparation method of the porous material using sol-gal process carried titanium dioxide, which is characterized in that including following Preparation step:
S01,6mL tetra-n-butyl titanate is measured, stirs in AR grades of ethanol solutions of lower instillation, adds inhibitor ice while stirring Acetic acid, until butyl titanate forms the colloidal solution of chelate;
S02, deionized water is added in the colloidal solution of preparation, so that colloidal particle is formed a kind of skeleton structure of opening, simultaneously It is slowly added to porous material, the porous material is porous material described in any one of claim 1-2, and the porous material Gel is formed until colloidal solution loses flowability for the activated alumina;
S03, at 100 DEG C by gel freeze-day with constant temperature >=for 24 hours, remove moisture, organic group and organic solvent in gel;
It is ground after S04, drying with mortar, is packed into crucible, be put into the Muffle furnace of nitrogen protection, muffle furnace rises to default temperature When spending, calcination time is kept the temperature, later the cooling porous material obtained using sol-gal process carried titanium dioxide of room temperature.
9. the preparation method of the porous material according to claim 8 using sol-gal process carried titanium dioxide, special Sign is:
In step S04, the preset temperature is at 450 DEG C or so, and Muffle furnace heating rate is 5 DEG C/min or so, heat preservation calcining Time is 4h.
CN201910118876.9A 2019-02-15 2019-02-15 A kind of porous material and preparation method using sol-gal process carried titanium dioxide Pending CN109647370A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN111249067A (en) * 2020-01-20 2020-06-09 福建恒安集团有限公司 Preparation method of deodorizing sanitary product
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