CN104607177A - Methanal purifying agent adopting visible light photocatalysis and preparation method of methanal purifying agent - Google Patents

Methanal purifying agent adopting visible light photocatalysis and preparation method of methanal purifying agent Download PDF

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CN104607177A
CN104607177A CN201410831921.2A CN201410831921A CN104607177A CN 104607177 A CN104607177 A CN 104607177A CN 201410831921 A CN201410831921 A CN 201410831921A CN 104607177 A CN104607177 A CN 104607177A
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pucherite
solution
purifying agent
visible light
titanium dioxide
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CN104607177B (en
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刘振森
何捷
聂卿
萧瑛
徐伟伟
崔敬轩
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China Building Materials Academy CBMA
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Abstract

The invention relates to a methanal purifying agent adopting visible light photocatalysis and a preparation method of the methanal purifying agent. The methanal purifying agent comprises pucherite and titanium dioxide, wherein the pucherite is loaded into the titanium dioxide, the mass ratio of the pucherite to the titanium dioxide is (0.6:100)-(0.67:100), and the crystalline phase of the pucherite is a monoclinic phase. According to the invention, the pucherite and the titanium dioxide are combined, through the synergy effect of the pucherite and the titanium dioxide, methanal can be effectively degraded within the ranges of the visible lights and ultraviolet rays, so that higher methanal purifying efficiency is achieved, and the methanal purifying agent is more suitable for practical usage.

Description

Formaldehyde purifying agent of visible light photocatalysis and preparation method thereof
Technical field
The present invention relates to a kind of cleanser and preparation method thereof, particularly a kind of formaldehyde purifying agent and preparation method thereof of visible light photocatalysis.
Background technology
Along with the raising of people's living standard and the variation of house decorative material, room air pollution also grows in intensity.As one of the key factor of room air pollution, formaldehyde can cause the organ such as respiratory tract, throat acute and chronic poisoning, reduces body immune function, causes neurasthenia, failure of memory.No. 153 " formaldehyde is carcinogenic " publications that the World Health Organization (WHO) issues are pointed out, formaldehyde not only can cause CARCINOMA OF THE NASAL CAVITY and nasal sinus cancer, have strongly but still insufficient evidence show can also leukemogenesis.Indoor formaldehyde derives from the material used in interior decoration or furniture, if glued board, chemical fibre carpet, wallpaper, core-board, paint, medium density fibre board (MDF), particieboard, wall covering fabric, coating, adhesive etc. are all to some extent containing formaldehyde or the chemical substance that can be analyzed to formaldehyde.These are residual or decompose formaldehyde out and can discharge in environment towards periphery gradually, and the longest release period can reach the more than ten years.Formaldehyde in purifying the air of a room has become major issue urgently to be resolved hurrily.
The principle of current formaldehyde purifying agent, adopts absorption method, chemical removal method, photocatalytic degradation method etc. more.At present, utilize the formaldehyde purifying agent of absorption method, the material mainly with bigger serfaces such as active carbon, modification slags is main, physical absorption formaldehyde.Utilize the purifying indoor formaldehyde agent of chemical removal method, mainly with amide derivatives, Polyphenols derivative (as vine polyphenol, lysine) is main component, generates other materials, realize the object of purifying formaldehyde with formaldehyde generation chemical reaction.Photocatalytic degradation method utilizes the energy with the material use light of semiconductor energy gap, organic matter and part inorganic matter is decomposed into the phenomenon of carbon dioxide and water.Compared with absorption method, chemical removal method etc., owing to having continues the effect, after degradation of formaldehyde, secondary pollution can not be produced, and to features such as the health of environment and people are harmless, the formaldehyde purifying agent exploitation of photocatalytic degradation method receives increasing concern.
Photochemical catalyst is the core of photocatalytic degradation.At present, purifying formaldehyde area research and application maximum photochemical catalysts be titanium dioxide.But due to TiO 2the wavelength of absorption maximum light is 387.5nm, i.e. TiO 2can only effectively absorb can by the ultraviolet portion (only accounting for 4% in sunshine) in light, therefore TiO 2class formaldehyde purifying agent cannot efficiency utilization visible ray, and this makes the efficiency of its purifying formaldehyde also lower.Although by chemisorbed or physical absorption Photoactive compounds (as Erythrosin B, thionine and transition metal oxide) in TiO 2the means such as surface, can expand its excitation wavelength range, but effect is but desirable not to the utmost.
Summary of the invention
The object of the invention is to, formaldehyde purifying agent of a kind of visible light photocatalysis and preparation method thereof is proposed, pucherite is combined with titanium dioxide, by the cooperative effect of the two, can effective degradation of formaldehyde in the scope of visible ray and ultraviolet light, thus obtain higher purifying formaldehyde efficiency, thus be more suitable for practicality.
The object of the invention is to be realized by following scheme, the formaldehyde purifying agent of a kind of visible light photocatalysis that the present invention proposes, it comprises pucherite and titanium dioxide, pucherite and TiO 2mass ratio be (0.6:100 ~ 0.67:100).Preferably, the crystalline phase of described pucherite is monoclinic phase.
Further, the formaldehyde purifying agent of above-mentioned visible light catalytic, described pucherite is prepared by following steps: bismuth salt and chelating agent are dissolved in acid and obtain the first solution;
The vanadate of solubility is dissolved in alkaline solution and obtains the second solution; Second solution is joined in the first solution, regulate Ph value to acid, obtain yellow suspension; Described yellow suspension is carried out hydrothermal treatment consists, then carries out Separation of Solid and Liquid, solid matter is washed, drying obtains Powdered pucherite.
Further, the formaldehyde purifying agent of above-mentioned visible light catalytic, also comprises: mixed with thickener, surfactant by described Powdered pucherite, and adjust ph is acid or neutral, obtains pucherite predispersion; Described titanium dioxide is joined in above-mentioned predispersion, described pucherite is loaded in titanium dioxide.Described vanadate is bismuth nitrate, and described chelating agent is EDTA, and described vanadate is ammonium vanadate; Described hydrothermal treatment consists is under air-proof condition, at 160-200 DEG C, keep 10-20 hour.Described pucherite is in the experiment of simulation rhodamine B degradation efficiency, and after its 90min, the degradation efficiency of rhodamine B is more than 95%.
The present invention also proposes a kind of preparation method of formaldehyde purifying agent of visible light photocatalysis, and it comprises the following steps:
Bismuth salt and chelating agent are dissolved in acid and obtain the first solution;
The vanadate of solubility is dissolved in alkaline solution and obtains the second solution;
Joined by second solution in the first solution, adjust ph, to acid, obtains yellow suspension;
Described yellow suspension is carried out hydrothermal treatment consists, then carries out Separation of Solid and Liquid, solid matter is washed, drying obtains Powdered pucherite;
Described Powdered pucherite is mixed with thickener, surfactant, and adjust ph is acid or neutral, obtains pucherite predispersion;
Titanium dioxide is joined in above-mentioned predispersion, makes described pucherite load in titanium dioxide, obtain the formaldehyde purifying agent of described visible light photocatalysis.
Further, the first described solution is: by Bi (NO 3) 35H 2o and EDTA is dissolved in the HNO of 2M successively under the condition of magnetic agitation 3in solution, wherein the mol ratio of EDTA and Bi is 0.2:1; The second described solution is: by NH 4vO 3be dissolved under the condition of magnetic agitation in the KOH of 2M; Just the second solution to join in the first solution and regulates pH=4, obtains yellow suspension.
Further, described predispersion is, Powdered pucherite is added in deionized water, after carrying out ultrasonic disperse, add successively hydroxyethylcellulose and neopelex, and regulate pH=7, obtain predispersion, wherein, pucherite and deionized water quality are than being 0.001-0.01%, the mass ratio of hydroxyethylcellulose and deionized water is 0.1-0.4%, and the mass ratio of neopelex and deionized water is 0.02-0.1%.In mass percentage, described predispersion accounts for the 25-75% of the formaldehyde purifying agent gross mass of visible light photocatalysis, pucherite and TiO 2mass ratio be (0.6:100 ~ 0.67:100).
Formaldehyde purifying agent of visible light photocatalysis of the present invention and preparation method thereof, at least has the following advantages:
Due to pucherite (BiVO 4, BVO) the wavelength of absorption maximum light be about 520nm (2.39ev), can comparatively TiO 2more extensively, effectively absorb visible ray, therefore, BVO is compound to existing TiO by the present invention 2in class formaldehyde purifying agent, it improves its purifying formaldehyde efficiency greatly, forms larger environmental benefit and economic benefit.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technological means of the present invention, and can be implemented according to the content of description, coordinates accompanying drawing to be described in detail as follows below with preferred embodiment of the present invention.
Accompanying drawing explanation
Fig. 1 is that the XRD collection of illustrative plates of BVO powder in example 1 and standard BiVO4 collection of illustrative plates contrast (JCPDS card number: 14-688)
Fig. 2 is XRD collection of illustrative plates and the standard BiVO of powder in example 2 4collection of illustrative plates contrast (JCPDS card number: 14-688)
Fig. 3 is powder simulating pollution thing (RhB) degradation efficiency comparison diagram; In figure, (a) is blank, (b) example 1 sample, (c) example 2 sample.
Fig. 4 is the effect diagram of different B VO and titanium dioxide mass ratio PARA FORMALDEHYDE PRILLS(91,95) purification efficiency; (a) 0% in figure, (b) 0.6:100, (c) 0.67:100.
Detailed description of the invention
For further setting forth the present invention for the technological means reaching predetermined goal of the invention and take and effect, below in conjunction with accompanying drawing and preferred embodiment, to the detailed description of the invention proposed according to the present invention, feature and effect thereof, be described in detail as follows.
Embodiment 1
The embodiment of the present invention 1 provides a kind of preparation method of formaldehyde purifying agent of visible light photocatalysis, and it comprises the following steps:
The preparation of Powdered pucherite:
Bismuth salt and chelating agent are dissolved in acid and obtain the first solution; The vanadate of solubility is dissolved in alkaline solution and obtains the second solution; Second solution is joined in the first solution, regulate Ph value to acid, obtain yellow suspension; Described yellow suspension is carried out hydrothermal treatment consists, then carries out Separation of Solid and Liquid, solid matter is washed, drying obtains Powdered pucherite.Further, the first described solution is: by Bi (NO 3) 35H 2o and EDTA is dissolved in the HNO of 2M successively under the condition of magnetic agitation 3in solution, wherein the mol ratio of EDTA and Bi is 0.2:1; The second described solution is: by NH 4vO 3be dissolved under the condition of magnetic agitation in the KOH of 2M; Just the second solution to join in the first solution and regulates pH=4, obtains yellow suspension.
The preparation of pucherite predispersion:
Described Powdered pucherite is mixed with thickener and surfactant, and adjust ph is neutral, obtains pucherite predispersion;
The preparation of formaldehyde purifying agent:
Titanium dioxide air purifying preparation of the prior art is joined in above-mentioned predispersion under the condition of magnetic agitation, and disperses within 10 minutes, to make described pucherite load in titanium dioxide at ultrasonic wave, pucherite and TiO later 2mass ratio be 0.6:100 ~ 0.67:100, obtain the formaldehyde purifying agent of the visible light photocatalysis of described stably dispersing.Further, in mass percentage, described predispersion accounts for the 25-75% of the formaldehyde purifying agent gross mass of visible light photocatalysis.
Following instance is the formaldehyde purifying agent preparing visible light photocatalysis according to the method for above-described embodiment 1.
Example 1
The preparation of step 1:BVO powder
By 0.01mol Bi (NO 3) 35H 2o and 0.002mol EDTA (EDTA:Bi=0.2:1) is dissolved in 15ml 2M HNO successively under the condition of magnetic agitation 3, obtain the first solution; By 0.01mol NH 4vO 3under the condition of magnetic agitation, be dissolved in 10ml 2M KOH obtain the second solution.Then, under the condition of magnetic agitation, the second dropwise is joined in the first solution, with 2M KOH or 2M HNO 3regulate pH=4, obtain yellow suspension.
Afterwards, yellow suspension to be transferred in water heating kettle (volume 100ml) and to seal, under inserting the condition of electric drying oven with forced convection 160 DEG C, keeping 20h.Finally, by suspension centrifugation in water heating kettle, and after cleaning 1 time with washed with de-ionized water 3 times, absolute alcohol, dry at electric drying oven with forced convection 60 DEG C and obtain yellow powder.
Can be found out by XRD collection of illustrative plates (Fig. 1), this yellow powder is the BVO (JCPDS card number: 14-688) of monoclinic phase, and this shows successfully to prepare BVO powder (particle diameter is 34-200nm).Simulating pollution thing (rhodamine B, RhB) degradation efficiency experimental result is as shown in Fig. 3 (b), after 90min, namely the degradation efficiency of RhB reaches 95.3%, far away higher than the blank degradation experiment (Fig. 3 (a)) not adding BVO powder.
Step 2: the preparation (relate to ratio in this part and be the mass ratio with deionized water) of predispersion
BVO powder is added in deionized water, the mass ratio of BVO and deionized water is 0.001%, after carrying out ultrasonic disperse 30min, the hydroxyethylcellulose (HEC) of 0.4% and the neopelex (LAS) of 0.02% is added successively, with 2M KOH or 2M HNO under the condition of magnetic agitation 3regulate pH=7, obtain predispersion.
Step 3: the preparation of visible ray formaldehyde purifying agent
In predispersion, (account for 75% of gross mass), add TiO 2(Beijing Si Narui Environmental Protection Technology Co., Ltd produces class air purifying preparation, containing TiO 2quality is 0.5%, TiO 2particle diameter is 10-60nm), wherein, predispersion and TiO 2class air purifying preparation mass ratio is 3:1, pucherite and TiO 2mass ratio be 0.6:100, carry out magnetic agitation 30min mixing, and after ultrasonic wave disperses 10 minutes, the formaldehyde purifying agent of the visible light photocatalysis of this example obtained.
According to purifying formaldehyde performance methodology in " function of purifying indoor air coating material purification property " (JC/T 1074-2008), the formaldehyde purifying agent of the visible light photocatalysis of example 1 gained is tested, after its 48h, purifying formaldehyde efficiency is 97.9% (as Suo Shi Fig. 4 (b)), is greater than TiO 2the purification efficiency of class air purifying preparation 85% (as Suo Shi Fig. 4 (a)).
Example 2
The preparation of step 1:BVO powder
By 0.01mol Bi (NO 3) 35H 2o and 0.005mol EDTA (EDTA:Bi=0.5:1) is dissolved in 15ml 2M HNO successively under the condition of magnetic agitation 3, the solution called after solution A obtained; By 0.01mol NH 4vO 3the solution called after B solution that 10ml 2M KOH obtains is dissolved under the condition of magnetic agitation.Then, under the condition of magnetic agitation, B solution is dropwise joined in solution A, with 2M KOH and 2M HNO 3regulate pH=7, obtain yellow suspension.
Afterwards, yellow suspension to be transferred in water heating kettle (volume 100ml) and to seal, under inserting the condition of electric drying oven with forced convection 200 DEG C, keeping 10h.Finally, by suspension centrifugation in water heating kettle, and after cleaning 1 time with washed with de-ionized water 3 times, absolute alcohol, dry at electric drying oven with forced convection 60 DEG C and obtain yellow powder.
Can be found out by XRD collection of illustrative plates (Fig. 2), this yellow powder is the BVO (JSPDS card number: 14-0688) of monoclinic phase, and this shows successfully to prepare BVO powder (particle diameter is 34-200nm).Simulating pollution thing (rhodamine B, RhB) degradation efficiency experimental result is as shown in Fig. 3 (c), after 90min, namely the degradation efficiency of RhB reaches 96.9%, far away higher than the blank degradation experiment (Fig. 3 (a)) not adding BVO powder.
Step 2: the preparation of predispersion
BVO powder is added in deionized water, the mass ratio of BVO and deionized water is 0.01%, after carrying out ultrasonic disperse 30min, under the condition of magnetic agitation, add hydroxyethylcellulose (HEC) and neopelex (LAS) successively, with 2M KOH and 2M HNO 3regulate pH=3, obtain predispersion, wherein, the mass ratio of hydroxyethylcellulose and deionized water is 0.1%, and the mass ratio of neopelex and deionized water is 0.1%.
Step 3: the preparation of visible ray formaldehyde purifying agent
TiO is added in predispersion 2(Beijing Si Narui Environmental Protection Technology Co., Ltd produces class air purifying preparation, containing TiO 2quality is 0.5%, TiO 2particle diameter is 10-60nm), wherein, predispersion and TiO 2class air purifying preparation mass ratio is 1:3, pucherite and TiO 2mass ratio be 0.67:100, carry out magnetic agitation 30min mixing, and after ultrasonic wave disperses 10 minutes, the formaldehyde purifying agent of the visible light photocatalysis of this example obtained.
According to purifying formaldehyde performance methodology in " function of purifying indoor air coating material purification property " (JC/T 1074-2008), performance test is carried out to the formaldehyde purifying agent of the visible light photocatalysis of this example, after its 48h, purifying formaldehyde efficiency is 96.1% (as Suo Shi Fig. 4 (c)), is greater than TiO 2the purification efficiency (as Suo Shi Fig. 4 (a)) of class air purifying preparation 85%.
Above embodiment shows, the formaldehyde purifying agent of the visible light photocatalysis prepared by said method, and it comprises pucherite and titanium dioxide, and described pucherite loads in titanium dioxide, and the crystalline phase of described pucherite is monoclinic phase.Wavelength due to the absorption maximum light of pucherite is about 520nm (2.39ev), can comparatively TiO 2more extensively, effectively absorb visible ray, more energy can be provided for cleanser of the present invention, thus degradation of formaldehyde institute energy requirement can be provided for titanium dioxide.Pucherite and titanium dioxide are combined with each other and are mutually supported by function each other by the present invention, thus obtain a kind of formaldehyde purifying agent exceeding any one matter of purification efficiency.
TiO described in above embodiment 2class air purifying preparation is prior art, can commercially purchase available with TiO 2for the cleanser of main functional component all can be applied in the present invention, and as the source of titanium dioxide in the formaldehyde purifying agent of visible light photocatalysis of the present invention.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, although the present invention discloses as above with preferred embodiment, but and be not used to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, make a little change when the technology contents of above-mentioned announcement can be utilized or be modified to the Equivalent embodiments of equivalent variations, in every case be the content not departing from technical solution of the present invention, according to any simple modification that technical spirit of the present invention is done above embodiment, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.

Claims (10)

1. a formaldehyde purifying agent for visible light photocatalysis, is characterized in that, comprises pucherite and titanium dioxide, and wherein, the mass ratio of pucherite and titanium dioxide is 0.6-0.67:100.
2. the formaldehyde purifying agent of visible light photocatalysis according to claim 1, is characterized in that, the crystalline phase of described pucherite is monoclinic phase.
3. the formaldehyde purifying agent of visible light catalytic according to claim 2, is characterized in that, described pucherite is prepared by following steps:
Bismuth salt and chelating agent are dissolved in acid and obtain the first solution;
The vanadate of solubility is dissolved in alkaline solution and obtains the second solution;
Joined by second solution in the first solution, adjust ph, to acid, obtains yellow suspension;
Described yellow suspension is carried out hydrothermal treatment consists, then carries out Separation of Solid and Liquid, solid matter is washed, drying obtains Powdered pucherite.
4. the formaldehyde purifying agent of visible light photocatalysis according to claim 3, is characterized in that, also comprises:
Described Powdered pucherite is mixed with thickener, surfactant, and adjust ph is acid or neutral, obtains pucherite predispersion;
Described titanium dioxide is joined in above-mentioned predispersion, described pucherite is loaded in titanium dioxide.
5. the formaldehyde purifying agent of visible light catalytic according to claim 3, is characterized in that, described vanadate is bismuth nitrate, and described chelating agent is EDTA, and described vanadate is ammonium vanadate; Described hydrothermal treatment consists is under air-proof condition, at 160-200 DEG C, keep 10-20 hour.
6. the formaldehyde purifying agent of the visible light photocatalysis according to any one of claim 1-5, is characterized in that, described pucherite is in the experiment of simulation rhodamine B degradation efficiency, and after its 90min, the degradation efficiency of rhodamine B is more than 95%.
7. a preparation method for the formaldehyde purifying agent of visible light photocatalysis, it comprises the following steps:
Bismuth salt and chelating agent are dissolved in acid and obtain the first solution;
The vanadate of solubility is dissolved in alkaline solution and obtains the second solution;
Second solution is joined in the first solution, regulate Ph value to acid, obtain yellow suspension;
Described yellow suspension is carried out hydrothermal treatment consists, then carries out Separation of Solid and Liquid, solid matter is washed, drying obtains Powdered pucherite;
Described Powdered pucherite is mixed with thickener, surfactant, and regulates Ph value for acid or neutral, obtain pucherite predispersion;
Titanium dioxide is joined in above-mentioned predispersion, makes described pucherite load in titanium dioxide, obtain the formaldehyde purifying agent of described visible light photocatalysis.
8. the preparation method of the formaldehyde purifying agent of visible light photocatalysis according to claim 7, is characterized in that,
The first described solution is: by Bi (NO 3) 35H 2o and EDTA is dissolved in the HNO of 2M successively under the condition of magnetic agitation 3in solution, wherein the mol ratio of EDTA and Bi is 0.2-0.5:1;
The second described solution is: by NH 4vO 3be dissolved under the condition of magnetic agitation in the KOH solution of 2M;
Just the second solution to join in the first solution and regulates pH=4, obtains yellow suspension.
9. the preparation method of the formaldehyde purifying agent of visible light photocatalysis according to claim 7, is characterized in that,
Described predispersion is, Powdered pucherite is added in deionized water, after carrying out ultrasonic disperse, add successively hydroxyethylcellulose and neopelex, and regulate pH=7, obtain predispersion, wherein, pucherite and deionized water quality are than being 0.001-0.01%, and the mass ratio of hydroxyethylcellulose and deionized water is 0.1-0.4%, and the mass ratio of neopelex and deionized water is 0.02-0.1%.
10. the preparation method of the formaldehyde purifying agent of the visible light photocatalysis according to any one of claim 7-9, wherein, in mass percentage, described predispersion accounts for the 25-75% of the formaldehyde purifying agent gross mass of visible light photocatalysis, pucherite and TiO 2mass ratio be 0.6-0.67:100.
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CN107335432A (en) * 2017-06-29 2017-11-10 天津城建大学 A kind of BiVO4/TiO2The preparation method of nucleocapsid composite photo-catalyst
CN107442103A (en) * 2017-08-25 2017-12-08 东北师范大学 The preparation method of pucherite/titanium dioxide composite film
CN110116013A (en) * 2019-05-15 2019-08-13 华东理工大学 Utilize the photocatalysis air-cleaning liquid and preparation method of sunlight and houselights

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CN106139895A (en) * 2016-08-15 2016-11-23 季红军 A kind of preparation method removing formaldehyde composite
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CN106861626A (en) * 2017-01-16 2017-06-20 华南理工大学 A kind of adsorption photochemical catalysis bifunctional material and preparation method thereof and the application in VOC Processing tecchnics
CN106861626B (en) * 2017-01-16 2020-01-14 华南理工大学 Adsorption-photocatalysis dual-function material, preparation method thereof and application thereof in volatile organic gas treatment process
CN107335432A (en) * 2017-06-29 2017-11-10 天津城建大学 A kind of BiVO4/TiO2The preparation method of nucleocapsid composite photo-catalyst
CN107335432B (en) * 2017-06-29 2020-02-14 天津城建大学 BiVO4/TiO2Preparation method of core-shell composite photocatalyst
CN107442103A (en) * 2017-08-25 2017-12-08 东北师范大学 The preparation method of pucherite/titanium dioxide composite film
CN110116013A (en) * 2019-05-15 2019-08-13 华东理工大学 Utilize the photocatalysis air-cleaning liquid and preparation method of sunlight and houselights

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