CN106824153A - TiO2The preparation method and applications of/Ludox - Google Patents

TiO2The preparation method and applications of/Ludox Download PDF

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CN106824153A
CN106824153A CN201710167999.2A CN201710167999A CN106824153A CN 106824153 A CN106824153 A CN 106824153A CN 201710167999 A CN201710167999 A CN 201710167999A CN 106824153 A CN106824153 A CN 106824153A
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solution
ludox
tio
preparation
iii
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CN106824153B (en
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刘玥
窦艳艳
秦贵棉
王聪民
吕晶晶
赵来群
赵富旺
张英
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Zhongyuan University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/08—Silica
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation 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
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation 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
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
    • B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/45—Gas separation or purification devices adapted for specific applications
    • B01D2259/4508—Gas separation or purification devices adapted for specific applications for cleaning air in buildings

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Environmental & Geological Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Biomedical Technology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • General Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Catalysts (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention belongs to catalyst field, and in particular to TiO2The preparation method and applications of/Ludox.Preparation method, step is as follows：By TiCl4In instillation 1L ultra-pure waters, and speed strong stirring in a water bath, obtain solution I；500mL ammonium chloride solutions and 500 mL hydrochloric acid solutions are thoroughly mixed, solution II is obtained；Solution II is added drop-wise in solution I, is mixed after being stood in baking oven, sodium silicate aqueous solution is added dropwise, while opening magnetic stirrer, as the pH6.9 7.1 of solution, stop titration, obtain solution III；Solution III is activated at room temperature, then with distilled water cyclic washing solution III, until the electrical conductivity of the supernatant of solution III is 0；Product is put into 4h is processed in baking oven, finally give TiO2/ Ludox solid particle.TiO prepared by the present invention2/ Ludox solid powder administers the application of indoor air pollutants as photochemical catalyst, and the removal effect of PARA FORMALDEHYDE PRILLS(91,95) gas is obvious.

Description

TiO2The preparation method and applications of/Ludox
Technical field
The invention belongs to catalyst field, and in particular to TiO2The preparation method and applications of/Ludox.
Background technology
The room air pollution caused by construction material, decorations, furniture etc. has been listed in global four rings of key One of border problem, it has also become a big killer of influence health of people.Therefore how to efficiently control indoor pollution, improve Interior Space Makings amount is problem anxious to be resolved at present.Treating indoor air pollution technology art can be broadly divided into by action principle：It is absorption method, quiet Electrodecontamination method, Ozonation and photocatalytic oxidation etc..Wherein nano material photocatalysis is room most with prospects at present Inner air-cleaning technology, but it is unable to the suspension and fine particulates in purify air；Catalyst micropore is easily grey simultaneously Dirt and particulate matter are blocked, and inactivate it.The present invention combines TiO2Problem present in photocatalytic process, and Ludox pair The suction-operated of pollutants in air, intends to TiO2It is modified, studies silicasol-supported TiO2The preparation and its photocatalysis of material The efficiency of indoor air pollutants.At present on silicasol-supported TiO2The preparation of material and its air pollutants are controlled indoors Application in reason is also rarely reported.
The content of the invention
The present invention utilizes silicasol-supported TiO for solution2Catalyst is prepared for the technical problem of room air pollution, it is public A kind of TiO is opened2The preparation method and applications of/Ludox.
To solve the above problems, the present invention uses following technical scheme：
TiO2The preparation method of/Ludox, step is as follows：
（1）By TiCl4In instilling 1 L ultra-pure waters, and stirred with the speed of 500 ~ 800 r/min in -5 DEG C ~ 1 DEG C water-bath 20min, obtains solution I；
（2）The hydrochloric acid solution of the ammonium chloride solution of the mol/L of 500 mL 0.1 ~ 0.5 and the mol/L of 500 mL 0.2 ~ 0.6 is complete Mixing, obtains solution II；
（3）Solution II is added drop-wise in solution I, is mixed after 1 ~ 2h is placed in 60 ~ 90 DEG C of baking oven, sodium metasilicate is added dropwise The aqueous solution, while open magnetic stirring apparatus stirred with the speed of 300 ~ 600 r/min, when pH 6.9-7.1 of solution, Stop titration, obtain solution III；
（4）Solution III is activated into 24 ~ 36h at room temperature, then with distilled water cyclic washing solution III, until the supernatant of solution III The electrical conductivity of liquid is 0；
（5）By step（4）In sediment be put into 4 h for the treatment of in 120 DEG C of baking oven, the white solid for finally giving is TiO2/ Ludox.
The step（1）Middle TiCl4Addition be 0.1 ~ 0.5 mol.
The step（3）The concentration of middle sodium silicate aqueous solution is 0.1 mol/L.
TiO2/ Ludox administers the application of indoor air pollutants as photochemical catalyst.
The beneficial effects of the present invention are：
（1）Under identical experiment condition, in the confined reaction device of given volume, the TiO of phase homogenous quantities is investigated2/ silicon is molten The degradation effect of glue and the commercially available titanium dioxide PARA FORMALDEHYDE PRILLS(91,95)s of P25：One group of independent ultraviolet light；One group adds 6 g TiO2/ silicon is molten Glue solid powder；One group adds 6g P25 titania powders.Concentration of formaldehyde is controlled in 2.5mg/m3, every 15min, 30min, 60min, 90min, 120min, 150min are measured by sampling the surplus of formaldehyde.Experimental result is as shown below, from figure As can be seen that under identical experiment condition, TiO2The removal effect of the addition PARA FORMALDEHYDE PRILLS(91,95) gas of/Ludox solid powder is obvious Better than P25, as shown in Figure 1.
（2）The TiO that the application is prepared2/ Ludox is easily recycled, and is not easily blocked, and sodium metasilicate is in strong basicity in water body, The sodium metasilicate of strong basicity is slowly dropped into the solution of acidity, on the one hand promotes mixed solution to decompose generation in the basic conditions Titanium dioxide, the sodium metasilicate of another aspect strong basicity can occur polymerisation in acid condition, energy and dioxy in polymerization process Change the surface hydroxyl and TiCl of titanium adsorption4The Ti produced in hydrolytic process（OH）4Generation is condensed dehydration, therefore made Standby TiO2/ Ludox is not the simple mixtures of titanium dioxide and Ludox, but the chemical bond of titanium dioxide and Ludox Even.
Brief description of the drawings
Fig. 1 is TiO2/ Ludox and P25 are except the design sketch of formaldehyde.
Specific embodiment
TiO2The preparation method of/Ludox, step is as follows：
（1）By TiCl4Instill 1L ultra-pure waters in, and in -5 DEG C ~ 1 DEG C water-bath with the speed of 500 ~ 800 r/min strongly Stirring 20min, obtains solution I；
（2）The hydrochloric acid solution of the ammonium chloride solution of the mol/L of 500 mL 0.1 ~ 0.5 and the mol/L of 500 mL 0.2 ~ 0.6 is complete Full mixing, obtains solution II；
（3）Solution II is added drop-wise in solution I, is mixed after 1 ~ 2h is placed in 60 ~ 90 DEG C of baking oven, sodium metasilicate water is added dropwise Solution, while open magnetic stirring apparatus being stirred with the speed of 300 ~ 600 r/min, as the pH 6.9-7.1 of solution, stops drop It is fixed, obtain solution III；
（4）Solution III is activated into 24 ~ 36h at room temperature, then with distilled water cyclic washing solution III, until the supernatant of solution III The electrical conductivity of liquid is 0；
（5）By step（4）In sediment be put into 4 h for the treatment of in 120 DEG C of baking oven, the white solid for finally giving is TiO2/ Ludox.
The step（1）Middle TiCl4Addition be 0.1 ~ 0.5mol.
The step（3）The concentration of middle sodium silicate aqueous solution is 0.1mol/L.
TiO2/ Ludox administers the application of indoor air pollutants as photochemical catalyst.
With reference to embodiment the present invention will be further explained explanation：
Embodiment 1
Step one：The TiCl of 0.5 mol4During instillation 1L is ultrapure, and stirred with the speed of 700 r/min in -5 DEG C of water-baths 20min；
Step 2：By the ammonium chloride solution of the mol/L of 500 mL 0.1 and the hydrochloric acid solution of the mol/L of 500 mL 0.2；
Step 3：The mixed aqueous solution is slowly dropped to the TiCl of step one gained4In the aqueous solution, by mixture at 90 DEG C Baking oven in place 1h, then be added dropwise concentration be 0.1 mol/L sodium silicate aqueous solution, when mixed liquor pH value be in 6.9 when Stop titration；
Step 4：Mixed liquor obtained by step 3 is activated into 24 h at room temperature；
Step 5：Electrical conductivity with distilled water cyclic washing to supernatant is zero；
Step 6：4 h are dried during sediment in step 5 is put into 120 DEG C of baking oven, and resulting white solid is TiO2/ Ludox solid particle.
Resulting TiO2The average pore size of/Ludox solid particle is 5.3 nm, and total pore volume is 0.425 cm3/ g, BET Specific surface area is 324.3m2/g。
Embodiment 2
Step one：The TiCl of 0.1 mol4During instillation 1L is ultrapure, and stirred with the speed of 500r/min in -3 DEG C of water-baths 20min；
Step 2：By the ammonium chloride solution of the mol/L of 500mL 0.5 and the hydrochloric acid solution of the mol/L of 500mL 0.6；
Step 3：The mixed aqueous solution is slowly dropped to the TiCl of step one gained4In the aqueous solution, by mixture at 70 DEG C Baking oven in place 2h, then be added dropwise concentration for 0.1mol/L sodium silicate aqueous solution, when mixed liquor pH value be in 7.0 when stop Only titrate；
Step 4：Mixed liquor obtained by step 3 is activated into 36h at room temperature；
Step 5：Electrical conductivity with distilled water cyclic washing to supernatant is zero；
Step 6：4h is dried during sediment in step 5 is put into 120 DEG C of baking oven, and resulting white solid is TiO2/ Ludox solid particle.
Resulting TiO2The average pore size of/Ludox solid particle is 5.6 nm, and total pore volume is 0.455 cm3/ g, BET Specific surface area is 344 m2/g。
Embodiment 3
Step one：The TiCl of 0.3 mol4During instillation 1L is ultrapure, and 20 are stirred with the speed of 800 r/min in 1 DEG C of water-bath min；
Step 2：By the ammonium chloride solution of the mol/L of 500 mL 0.3 and the hydrochloric acid solution of the mol/L of 500 mL 0.4；
Step 3：The mixed aqueous solution is slowly dropped to the TiCl of step one gained4In the aqueous solution, by mixture 60 DEG C baking oven in place 1.5 h, then be added dropwise concentration be 0.1 mol/L sodium silicate aqueous solution, when the pH value of mixed liquor is in Stop titration when 6.9；
Step 4：Mixed liquor obtained by step 3 is activated into 30h at room temperature；
Step 5：Electrical conductivity with distilled water cyclic washing to supernatant is zero；
Step 6：4h is dried during sediment in step 5 is put into 120 DEG C of baking oven, and resulting white solid is TiO2/ Ludox solid particle.
Resulting TiO2The average pore size of/Ludox solid particle is 5.5nm, and total pore volume is 0.435 cm3/ g, BET ratio Surface area is 354.3 m2/g。
Embodiment 4
Step one：The TiCl of 0.3 mol4During instillation 1L is ultrapure, and stirred with the speed of 700r/min in -2 DEG C of water-baths 20min；
Step 2：By the ammonium chloride solution of the mol/L of 500mL 0.2 and the hydrochloric acid solution of the mol/L of 500mL 0.5；
Step 3：The mixed aqueous solution is slowly dropped to the TiCl of step one gained4In the aqueous solution, by mixture at 80 DEG C Baking oven in place 2h, then be added dropwise concentration for 0.1mol/L sodium silicate aqueous solution, when mixed liquor pH value be in 7.1 when stop Only titrate；
Step 4：Mixed liquor obtained by step 3 is activated into 30h at room temperature；
Step 5：Electrical conductivity with distilled water cyclic washing to supernatant is zero；
Step 6：4h is dried during sediment in step 5 is put into 120 DEG C of baking oven, and resulting white solid is TiO2/ Ludox solid particle.
Resulting TiO2The average pore size of/Ludox solid particle is 5.7 nm, and total pore volume is 0.435 cm3/ g, BET Specific surface area is 354.3m2/g。
Embodiment 5
Step one：The TiCl of 0.3 mol4During instillation 1L is ultrapure, and stirred with the speed of 750r/min in -2 DEG C of water-baths 20min；
Step 2：By the ammonium chloride solution of the mol/L of 500mL 0.2 and the hydrochloric acid solution of the mol/L of 500mL 0.5；
Step 3：The mixed aqueous solution is slowly dropped to the TiCl of step one gained4In the aqueous solution, by mixture at 90 DEG C Baking oven in place 1h, then be added dropwise concentration for 0.1mol/L sodium silicate aqueous solution, when mixed liquor pH value be in 7.1 when stop Only titrate；
Step 4：Mixed liquor obtained by step 3 is activated into 30h at room temperature；
Step 5：Electrical conductivity with distilled water cyclic washing to supernatant is zero；
Step 6：4h is dried during sediment in step 5 is put into 120 DEG C of baking oven, and resulting white solid is TiO2/ Ludox solid particle.
Resulting TiO2The average pore size of/Ludox solid particle is 5.8 nm, and total pore volume is 0.465 cm3/ g, BET Specific surface area is 360.3m2/g。
Embodiment 6
Step one：The TiCl of 0.4 mol4During instillation 1L is ultrapure, and stirred with the speed of 850r/min in -4 DEG C of water-baths 20min；
Step 2：By the ammonium chloride solution of the mol/L of 500mL 0.3 and the hydrochloric acid solution of the mol/L of 500mL 0.5；
Step 3：The mixed aqueous solution is slowly dropped to the TiCl of step one gained4In the aqueous solution, by mixture at 90 DEG C Baking oven in place 1h, then be added dropwise concentration for 0.1mol/L sodium silicate aqueous solution, when mixed liquor pH value be in 7.1 when stop Only titrate；
Step 4：Mixed liquor obtained by step 3 is activated into 30h at room temperature；
Step 5：Electrical conductivity with distilled water cyclic washing to supernatant is zero；
Step 6：4h is dried during sediment in step 5 is put into 120 DEG C of baking oven, and resulting white solid is TiO2/ Ludox solid particle.
Resulting TiO2The average pore size of/Ludox solid particle is 5.6 nm, and total pore volume is 0.465 cm3/ g, BET Specific surface area is 360.3m2/g。

Claims (4)

1.TiO2The preparation method of/Ludox, it is characterised in that step is as follows：
（1）By TiCl4In instillation 1L ultra-pure waters, and 20 are stirred with the speed of 500 ~ 800 r/min in -5 DEG C ~ 1 DEG C water-bath Min, obtains solution I；
（2）The hydrochloric acid solution of the ammonium chloride solution of the mol/L of 500 mL 0.1 ~ 0.5 and the mol/L of 500 mL 0.2 ~ 0.6 is complete Mixing, obtains solution II；
（3）Solution II is added drop-wise in solution I, is mixed after 1 ~ 2 h is placed in 60 ~ 90 DEG C of baking oven, sodium metasilicate is added dropwise The aqueous solution, while open magnetic stirring apparatus being stirred with the speed of 300 ~ 600 r/min, as the pH 6.9-7.1 of solution, stops Titration, obtains solution III；
（4）Solution III is activated into 24 ~ 36h at room temperature, then with distilled water cyclic washing solution III, until the supernatant of solution III Electrical conductivity be 0；
（5）By step（4）In sediment be put into treatment 4h, the white solid for finally giving as TiO in 120 DEG C of baking oven2/ Ludox.
2. the preparation method of TiO2/ Ludox as claimed in claim 1, it is characterised in that：The step（1）Middle TiCl4Plus Enter amount for 0.1 ~ 0.5mol.
3. TiO as claimed in claim 12The preparation method of/Ludox, it is characterised in that：The step（3）Middle sodium metasilicate water The concentration of solution is 0.1mol/L.
4.TiO2/ Ludox administers the application of indoor air pollutants as photochemical catalyst.
CN201710167999.2A 2017-03-21 2017-03-21 TiO2Preparation method and application of silica sol Expired - Fee Related CN106824153B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006346645A (en) * 2005-06-20 2006-12-28 Azumi Roshi Kk Metal filter and its manufacturing method
CN101288835A (en) * 2008-06-02 2008-10-22 大连工业大学 TiO2-SiO2 compound aerogel and its preparation method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006346645A (en) * 2005-06-20 2006-12-28 Azumi Roshi Kk Metal filter and its manufacturing method
CN101288835A (en) * 2008-06-02 2008-10-22 大连工业大学 TiO2-SiO2 compound aerogel and its preparation method

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
X FUDENG: "Enhanced Photocatalytic Performance of Titania-Based Binary Metal Oxides: TiO2/SiO2 and TiO2/ZrO2", 《ENVIRON. SCI. TECHNOL.》 *
杜凤: "高耐候TiO2表面包覆SiO2的研究", 《山东化工》 *
甘礼华等: "TiO2/SiO2气凝胶对亚甲基蓝降解的光催化活性", 《同济大学学报（自然科学版）》 *

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