CN103756467A - Preparation method of environment-friendly interior wall top coating for preforming catalytic degradation on formaldehyde in air during photocatalysis and chemical oxidation - Google Patents
Preparation method of environment-friendly interior wall top coating for preforming catalytic degradation on formaldehyde in air during photocatalysis and chemical oxidation Download PDFInfo
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- CN103756467A CN103756467A CN201410013035.9A CN201410013035A CN103756467A CN 103756467 A CN103756467 A CN 103756467A CN 201410013035 A CN201410013035 A CN 201410013035A CN 103756467 A CN103756467 A CN 103756467A
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Abstract
The invention provides a preparation method of an environment-friendly interior wall top coating for preforming catalytic degradation on formaldehyde in air during photocatalysis and chemical oxidation. The environment-friendly interior wall top coating comprises a formaldehyde degrading agent capable of performing catalytic degradation on formaldehyde, wherein the formaldehyde degrading agent is prepared by using a precipitation method. The formaldehyde degrading agent is a titanium dioxide powder body which has a certain crystal form and contains molybdenum trioxide and other metal oxides on the surface. The environment-friendly interior wall top coating is higher in acid catalytic activity, is used in acid catalysis reaction, and is also suitable for catalytic oxidation degradation of the formaldehyde. The powder body is safe, non-volatile and pollution-free. The environment-friendly interior wall top coating provided by the invention is environment-friendly and free from pollution; the degradation rate to the formaldehyde in indoor air can reach 73.3 percent.
Description
Technical field
The invention belongs to building material technical field, be specifically related to a kind of high-efficiency environment friendly, photochemical catalysis and chemical oxidation and carry out the preparation method of the environmental protection wall surface paint of formaldehyde in catalyzed degradation air simultaneously.
Background technology
Wall paint as coating is one of indispensable material of upholstery.Conventionally wall paint is by composite compositions such as tackiness agent, water, white filler, solidifying agent, mould inhibitors, to reach the object of indoor beautifying.
Except decoration and beautifying functions, Multifunction wall finish paint is also developed gradually, and major function is disinfection, absorbs ultraviolet ray, absorbs the effects such as obnoxious flavour.
Formaldehyde is to produce the requisite raw materials such as synthetic resins, paint, regenerated fiber, artificial board.In indoor environment of today, along with various finishing equipment, the use of decorating materials, take formaldehyde, benzene class is that main organic compound also occurs thereupon.Show according to the study, formaldehyde content exceeds standard and can cause the mankind's nasopharyngeal carcinoma, CARCINOMA OF THE NASAL CAVITY and nasal sinus cancer, and can cause leukemia.In a word, for healthy, the excessive absorption of any material all can make the person suffer damage, and the organic pollutants such as benzene-like compounds and formaldehyde are because it exists and easily make people ignore their hazardness with the form of gas in air.Therefore develop a kind of environmental protection wall surface paint, its objective is the formaldehyde in degraded room air, protection HUMAN HEALTH.
The method that reduces at present formaldehyde content in air mainly contains two kinds of physisorphtion and photodegradation methods.The method of physical adsorption is to use porous material, as charcoal, gac etc., utilizes its structural porousness absorption formaldehyde.This kind of method adsorption efficiency is low, and the state that reaches capacity after certain absorption content that arrives no longer adsorbs.Photodegradation method is that the material that adopts titanium dioxide etc. to have semiconductor structure completes oxidation operation under UV-irradiation.But this kind of method is because it absorbs light source in ultraviolet region, and seldom, degradation effect is restricted the UV-light in daylight.
Patent publication No. CN102382562A adopts photodegradative principle that Nano titanium dioxide is joined in clear lacquer and carries out degradation of formaldehyde, and its titanium dioxide does not process.Patent publication No. CN101874978A joins titanium dichloride load in indoor paint on diatomite, for degradation of formaldehyde, has emphasized that diatomite increases the method for specific surface area.Patent publication No. CN102241943A adopts titanium dioxide to add degradation of formaldehyde in coating to, and it is to be less than 100 nanometers that photodegradable aid is required.Patent publication No. CN102828447A and CN102686311A have announced titanium dioxide and Tungsten oxide 99.999, manganese oxide are the light-sensitive catalyst degradation of formaldehyde of the bimetal component of combination.Patent publication No. CN1772353A is used four-needle-like zinc oxide, and mixes and use degradation of formaldehyde with oxide compounds such as zirconium, silicon, aluminium, magnesium.Patent publication No. CN1772353A on natural micropore metal raw ore, prepares the material of photodegradation formaldehyde by titanium dichloride load.Patent publication No. CN102806077A adopts carried titanium dioxide and stannic oxide on recessed soil, and photocatalytic mechanism is analyzed, but does not provide concrete carrying method.
Above method common ground is to utilize the susceptibility to light of titanium dioxide to carry out degradation of formaldehyde, is single photodegradative method.
Titanium dioxide is a kind of semi-conductor, in molecular orbital(MO), there is full valence band and empty conduction band, be subject to the electronics in valence band after rayed and will be excited to conduction band, at conduction band, form active high electronics, and the valence band that loses electronics can form a positively charged hole.The active electrons of titanium dioxide surface and hole have very high activity, can form hydroxide radical free radical with water or hydroxyl, and free radical can be oxidized most organism.
What can make titanic oxide electronic transition must have enough energy, and wavelength must be less than 387nm.Nature light wavelength is generally 380nm～780nm, and the less energy of light wavelength is higher, and only purpuric light 380～440nm just can make titanium dioxide play katalysis, and other most light do not have effect.In order to make the transition of electron of titanium dioxide, add the minimum wavelength that other components can change transition.Conventionally add zinc oxide, Cadmium Sulfide, ferric oxide Tungsten oxide 99.999 and manganese oxide, patent publication No. CN102686311A has been used manganese oxide.
Patent publication No. CN102827523A has adopted the method for chemical reaction to carry out degradation of formaldehyde.They have adopted and in wall paint, have added urea, and that utilizes that urea and aldehyde generates semicarbazone reacts to remove airborne formaldehyde.This method does not have Degradation Formaldehyde, but has generated another kind of chemical substance.
Summary of the invention
The object of the invention is to provide a kind of titanium dioxide of modifying with complex metal oxides, and as Degradation Formaldehyde, agent carrys out the degrade environmental protection wall surface paint of formaldehyde in air of photochemical catalysis and chemical oxidation dual catalytic.This Degradation Formaldehyde agent be take titanium hydroxide as matrix, take molybdic oxide and other metal oxides titanium dioxide to be modified as improving agent.This wall paint ventilation property, resistance to deterioration, water tolerance, hardness are good, can continue by photochemical catalysis and the chemical oxidation formaldehyde in air of degrading, nontoxic pollution-free simultaneously.
The object of the invention is to be achieved by the following technical programs:
Photochemical catalysis and chemical oxidation carry out a preparation method for the environment protection interior wall finish paint of formaldehyde in catalyzed degradation air simultaneously, it is characterized in that, by mass percentage, by following component, are prepared from:
The preparation method of described Degradation Formaldehyde agent is:
1. titanium tetrachloride is joined in deionized water, drip ammoniacal liquor and regulate pH to 9～11, under the condition of 0～25 ℃, sedimentation is 10～20 hours, filtration under diminished pressure, to chloride ion-containing not, is dried to constant weight under 110 ℃ of conditions with deionized water washing leaching cake, cross 200 mesh sieves, obtain white titanium hydroxide powder;
2. first in the sulphuric acid soln of 1～1.5mol/L, add ammonium molybdate, after treating that ammonium molybdate all dissolves, the whiter titanium hydroxide powder that adds step 1. to make, finally add improving agent, stir 4 hours;
3. the product 2. step being obtained is put into chamber type electric resistance furnace heating and is concentrated into absence of liquid, and under the condition of 500～600 ℃, roasting is 3～4 hours, obtains Degradation Formaldehyde agent;
Described ammonium molybdate, titanium hydroxide are 1～5:100 according to mol ratio;
The mol ratio of improving agent and ammonium molybdate is 1～6:3;
Described improving agent is the mixture of any one or two kinds in the oxide compound, nitrate, vitriol, metal acid-salt of Ta, W, Cr, Sm, Eu, Ni, Ce, Mn, Zn;
When improving agent is in the oxide compound, nitrate, vitriol, metal acid-salt of Ta, W, Cr, Sm, Eu, Ni, Ce, Mn, Zn during the mixture of any two kinds, in described improving agent, the mol ratio of two metal ion species is 1～5:1;
Described emulsion is any one in pure-acrylic emulsion, benzene emulsion, acrylate and vinyl acetate emulsion;
Described environment protection interior wall finish paint preparation method is:
A) water is added in reactor, with low speed, 300～600r/min stirs, and slowly adds Mierocrystalline cellulose, and then middling speed 800～1200r/min disperses, and disperses 20 minutes;
B): progressively add propylene glycol, titanium dioxide, Degradation Formaldehyde agent, calcium carbonate, kaolin, talcum powder, dispersion agent, defoamer, 1500～2000r/min dispersed with stirring is 30 minutes at a high speed.；
C): progressively add emulsion, defoamer, thickening material, sterilant, flow agent and wetting agent, 1500～2000r/min stirs and within 30 minutes, obtains environment protection interior wall finish paint at a high speed.
Beneficial effect of the present invention is:
1) prepared a kind of interior finish of degradable formaldehyde, this paint contains a kind of photochemical catalysis Degradation Formaldehyde agent of chemical catalytic oxidation degradation of formaldehyde simultaneously.This Degradation Formaldehyde agent is owing to having added molybdic oxide and other metal oxides, with and the feature of concentrated cocrystallization (its crystal formation also has its special structure, the titanium dioxide of anatase octahedrite and rutile mixing crystal formation, be mainly Detitanium-ore-type, cannot explain at present these special crystal formations), make the transition of electron wavelength of titanium dioxide elongated, cause a greater variety of light to have stimulation effect to carry out degradation of formaldehyde to titanium dioxide, therefore the utilization ratio that, has improved visible ray reaches the object of efficient degradation formaldehyde;
2) XRD of this Degradation Formaldehyde agent shows to exist special crystal phase structure and acidity, makes formaldehyde can carry out with this understanding chemical catalytic oxidation degraded.The mode of this degradation of formaldehyde with by means such as titanium dioxide or working loads, come degradation of formaldehyde to compare obvious progress merely;
3) with the indoor wall finish paint that this Degradation Formaldehyde agent configures, there are environmental protection, efficient effect.
Accompanying drawing explanation
5, the total accompanying drawing of the present invention, wherein:
The Degradation Formaldehyde agent degradation of formaldehyde efficiency diagram of preparation in Fig. 1 embodiment 1～4;
The XRD spectra of the Degradation Formaldehyde agent of preparation in Fig. 2 embodiment 1～4;
The uv drs spectrogram of the Degradation Formaldehyde agent of preparation in Fig. 3 embodiment 1～4;
The ammonia temperature programming adsorption/desorption figure of the Degradation Formaldehyde agent of preparation in Fig. 4 embodiment 1～4;
Scanning electron microscope (SEM) photograph (the a:TiO of the Degradation Formaldehyde agent of preparation in Fig. 5 embodiment 1～4
2, b:TiO
2-MoO
3-MnO, c:TiO
2-MoO
3, d:TiO
2-MoO
3-CrO
3).
Embodiment
In embodiment, raw materials used source is as follows:
Embodiment 1
(1) preparation of Degradation Formaldehyde agent
20g titanium tetrachloride is dissolved in 50ml deionized water, under 20 ℃ of conditions, drips ammoniacal liquor and regulate pH to 9～11.Under 20 ℃ of conditions, sedimentation is 20 hours, filtration under diminished pressure.To chloride ion-containing not, dry with deionized water washing leaching cake, sieve, obtain white titanium hydroxide powder ().
4g ammonium molybdate is dissolved in to 20ml(1mol/L) sulfuric acid in, add 10g titanium hydroxide, then add 0.4g chromium trioxide, stir 4 hours.Heating is concentrated into liquid and disappears, and with roasting in 550 ℃ of chamber type electric resistance furnaces 3 hours, obtains Degradation Formaldehyde agent.Adopt X-ray diffraction, uv drs, ammonia temperature programming adsorption/desorption and scanning electron microscope to detect, result is shown in respectively Fig. 2,3,4 and 5.
(2) modulation of indoor wall finish paint and test
Deionized water 250g is poured in the reactor that stirring is housed, low speed 300～600r/min stirs and adds 3g Mierocrystalline cellulose, and middling speed disperses to obtain for 20 minutes mixture.20g propylene glycol, 180g titanium dioxide, the agent of 70g Degradation Formaldehyde, 60g calcium carbonate, 40g kaolin, 60g talcum powder, 3g dispersion agent Orotan731,2g defoamer 618F are joined in reactor, and 1500～2000r/min stirs 30 minutes at a high speed.Add 2g defoamer 618F, vinegar 300g acrylic emulsion, 2g thickening material TT935,2g wetting agent X405,2g flow agent RM2020 and 3g sterilant K20,1500～2000r/min stirs 30 minutes at a high speed, obtains the indoor wall finish paint of degradable formaldehyde.
The wall paint making is coated on cement matrix, carries out appearance of film, surface drying time, alkali resistance, low-temperature stability, contrast ratio, scrub resistance experiment (GB/T9756-2001), experimental result is in Table 1.
Table 1 paint film use properties detects table
| Performance Detection | Test-results |
| State in container | Be uniformly mixed rear without lump |
| Appearance of film | Appearance of film is normal |
| Surface drying time | 1 hour |
| Alkali resistance | 24 hours without abnormal |
| Low- |
3 circulations are without rotten |
| Contrast ratio | 0.97 |
| Abrasion resistance | 1200 times |
(3) detection of Degradation Formaldehyde
The wall paint making is coated on 20mm * 90mm sheet glass to dry being placed in the encloses container of 2500ml.Trioxymethylene is heated to thawing and makes formaldehyde gas, according to the concentration of 30mg/L, with syringe, be injected in encloses container.Timing sampling product, according to the content of GB/T15516-1955 measurement formaldehyde, experimental result as shown in Figure 1.Result shows that after 3 days, recording gained Degradation Formaldehyde rate is 73.3%.
4g ammonium molybdate is dissolved in to 20ml(1mol/L) sulfuric acid in, add 10g titanium hydroxide, then add 0.4g manganous sulfate, stir 4 hours.With chamber type electric resistance furnace heating, be concentrated into liquid and disappear, in 550 ℃, roasting is 3 hours, obtains Degradation Formaldehyde agent.Adopt X-ray diffraction, uv drs and scanning electron microscope to detect, result is shown in respectively Fig. 2,3,4 and 5.
Method according to embodiment 1 is made wall paint, and the effect of degradation of formaldehyde is shown in Fig. 1, and after 3 days, recording gained Degradation Formaldehyde rate is 70.7%.
4g ammonium molybdate is dissolved in to 20ml(1mol/L) sulfuric acid in, add 10g titanium hydroxide, stir 4 hours.With chamber type electric resistance furnace heating, be concentrated into liquid and disappear, in 550 ℃, roasting is 3 hours, obtains Degradation Formaldehyde agent.Adopt X-ray diffraction, uv drs and scanning electron microscope to detect, result is shown in respectively Fig. 2,3,4 and 5.
Method according to embodiment 1 is made wall paint, and the effect of degradation of formaldehyde is shown in Fig. 1, and after 3 days, recording gained Degradation Formaldehyde rate is 40.2%.
At 20ml(1mol/L) sulfuric acid in, add 10g titanium hydroxide, stir 4 hours.With chamber type electric resistance furnace heating, be concentrated into liquid and disappear, in 550 ℃, roasting is 3 hours, obtains Degradation Formaldehyde agent.Adopt X-ray diffraction, uv drs, ammonia temperature programming adsorption/desorption and scanning electron microscope to detect, result is shown in respectively Fig. 2,3,4 and 5.
Method according to embodiment 1 is made wall paint, and the effect of degradation of formaldehyde is shown in Fig. 1, and after 3 days, recording gained Degradation Formaldehyde rate is 20.5%.
Embodiment 5
4g ammonium molybdate is dissolved in to 20ml(1mol/L) sulfuric acid in, add 10g titanium hydroxide, then add 0.4g single nickel salt, stir 4 hours.With chamber type electric resistance furnace heating, be concentrated into liquid and disappear, in 600 ℃, roasting is 3 hours, obtains Degradation Formaldehyde agent.
Method according to embodiment 1 is made wall paint, and after 3 days, recording gained Degradation Formaldehyde rate is 65.4%.
Embodiment 6
4g ammonium molybdate is dissolved in to 20ml(1mol/L) sulfuric acid in, add 10g titanium hydroxide, then add metal oxide, nitrate, vitriol or the metal acid-salt of a kind of or two kinds of 0.005mol, stir 4 hours.With chamber type electric resistance furnace heating, be concentrated into liquid and disappear, in 600 ℃, roasting is 3 hours, obtains Degradation Formaldehyde agent.
Method according to embodiment 1 is made wall paint, and experimental result is in Table 2, and Degradation Formaldehyde agent prepared by the inventive method has mixing crystalline structure (anatase octahedrite and rutile mixing crystal formation, Detitanium-ore-type is main).
Table 2 Degradation Formaldehyde agent degradation of formaldehyde efficiency table
| Numbering | Component | Degradation rate |
| 1 | TiO 2-MoO 3-ZnO | 70.5% |
| 2 | TiO 2-MoO 3-ZnO-Ta 2O 5 | 71.3% |
| 3 | TiO 2-MoO 3-ZnO-WO 3 | 72.6% |
| 4 | TiO 2-MoO 3-ZnO-NiO | 72.1% |
| 5 | TiO 2-MoO 3-WO 3 | 68.7% |
| 6 | TiO 2-MoO 3-WO 3-NiO | 69.3% |
| 7 | TiO 2-MoO 3-MnO 2-CeO 2 | 69.8% |
| 8 | TiO 2-MoO 3-ZrO 2-La 2O 3 | 68.9% |
Embodiment 7
4g ammonium molybdate is dissolved in to 20ml(1mol/L) sulfuric acid in, add 8g anatase titanium dioxide and 2g titanium hydroxide, then add metal oxide, nitrate, vitriol or metal acid-salt, stir 4 hours.With chamber type electric resistance furnace heating, be concentrated into liquid and disappear, in 600 ℃, roasting is 3 hours, obtains Degradation Formaldehyde agent.
Method according to embodiment 1 is made wall paint, records gained Degradation Formaldehyde rate and reach in Table 3 after 3 days.
With titanium tetrachloride, be that raw material is prepared Degradation Formaldehyde agent price, and the industrial goods of Detitanium-ore-type are then through processing, just can obtain with ore extraction, price is very cheap.We are carrier with anatase titanium dioxide industrial goods, dissolve in part titanium hydroxide as titanium source in acid, and then concentrated and roasting makes titanium and other metals in titanium dioxide surface cocrystallization.Observe the effect of its degradation of formaldehyde.
Table 3 Degradation Formaldehyde agent degradation of formaldehyde efficiency table
| Numbering | Component | Degradation rate (%) |
| 1 | TiO 2-MoO 3-NiO | 55.4 |
| 2 | TiO 2-MoO 3-WO 3 | 53.2 |
| 3 | TiO 2-MoO 3-ZnO | 56.7 |
| 4 | TiO 2-MoO 3-Ta 2O 5 | 53.3 |
| 5 | TiO 2-MoO 3-NiO-WO 3 | 57.7 |
| 6 | TiO 2-MoO 3-ZnO-Ta 2O 5 | 57.2 |
| 7 | TiO 2-MoO 3-NiO-Ta 2O 5 | 58.2 |
| 8 | TiO 2-MoO 3-ZnO-WO 3 | 57.0 |
| 9 | TiO 2-MoO 3-Ta 2O 5-WO 3 | 54.1 |
4g ammonium molybdate is dissolved in to 20ml(1mol/L) sulfuric acid in, add 8g rutile titanium dioxide and 2g titanium hydroxide, then add metal oxide, nitrate, vitriol or metal acid-salt, stir 4 hours.With roasting in 600 ℃ of chamber type electric resistance furnaces 3 hours, obtain Degradation Formaldehyde agent.
Similar to embodiment 7, rutile titanium dioxide industrial goods are carrier.Observe the effect of its degradation of formaldehyde.
Method according to embodiment 1 is made wall paint, records gained Degradation Formaldehyde rate and reach in Table 4 after 3 days.
Table 4 Degradation Formaldehyde agent degradation of formaldehyde efficiency table
Comparative example 1
Rutile titanium dioxide, anatase titanium dioxide are made to wall paint according to the method for embodiment 1, after 3 days, record gained Degradation Formaldehyde rate and be respectively 10.8% and 25.3%.
Comparative example 2
The molten 50ml of 20g titanium tetrachloride, in deionized water, is added to 50g diatomite, at 20 ℃, drip ammoniacal liquor, regulate pH to 9～11.Under 20 ℃ of conditions, sedimentation is 20 hours, filtration under diminished pressure.To chloride ion-containing not, dry with deionized water washing leaching cake, sieve, obtain the diatomite of white titanium hydroxide load.
By the roasting 3 hours in 600 ℃ of the titanium hydroxide of load, obtain Degradation Formaldehyde agent.Method according to embodiment 1 is made wall paint, and after 3 days, recording gained Degradation Formaldehyde rate is 27.1%.
Claims (1)
1. photochemical catalysis and chemical oxidation carry out a preparation method for the environment protection interior wall finish paint of formaldehyde in catalyzed degradation air simultaneously, it is characterized in that, by mass percentage, by following component, are prepared from:
The preparation method of described Degradation Formaldehyde agent is:
1. titanium tetrachloride is joined in deionized water, drip ammoniacal liquor and regulate pH to 9～11, under the condition of 0～25 ℃, sedimentation is 10～20 hours, filtration under diminished pressure, to chloride ion-containing not, is dried to constant weight under 110 ℃ of conditions with deionized water washing leaching cake, cross 200 mesh sieves, obtain white titanium hydroxide powder;
2. first in the sulphuric acid soln of 1～1.5mol/L, add ammonium molybdate, after treating that ammonium molybdate all dissolves, the whiter titanium hydroxide powder that adds step 1. to make, finally add improving agent, stir 4 hours;
3. the product 2. step being obtained is put into chamber type electric resistance furnace heating and is concentrated into absence of liquid, and under the condition of 500～600 ℃, roasting is 3～4 hours, obtains Degradation Formaldehyde agent;
Described ammonium molybdate, titanium hydroxide are 1～5:100 according to mol ratio;
The mol ratio of improving agent and ammonium molybdate is 1～6:3;
Described improving agent is the mixture of any one or two kinds in the oxide compound, nitrate, vitriol, metal acid-salt of Ta, W, Cr, Sm, Eu, Ni, Ce, Mn, Zn;
When improving agent is in the oxide compound, nitrate, vitriol, metal acid-salt of Ta, W, Cr, Sm, Eu, Ni, Ce, Mn, Zn during the mixture of any two kinds, in described improving agent, the mol ratio of two metal ion species is 1～5:1;
Described emulsion is any one in pure-acrylic emulsion, benzene emulsion, acrylate and vinyl acetate emulsion;
Described environment protection interior wall finish paint preparation method is:
A): first water is added in reactor, with low speed, 300～600r/min stirs, slowly add Mierocrystalline cellulose, then middling speed 800～1200r/min disperses, and disperses 20 minutes;
B): in reactor, progressively add propylene glycol, titanium dioxide, Degradation Formaldehyde agent, calcium carbonate, kaolin, talcum powder, dispersion agent, defoamer again, 1500～2000r/min dispersed with stirring is 30 minutes at a high speed;
C): progressively add emulsion, defoamer, thickening material, sterilant, flow agent and wetting agent, 1500～2000r/min stirs and within 30 minutes, obtains environment protection interior wall finish paint.
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| CN107828288A (en) * | 2017-11-07 | 2018-03-23 | 河北晨阳工贸集团有限公司 | A kind of anti-formaldehyde type interior wall sealing wax and preparation method thereof |
| CN108465473A (en) * | 2018-03-13 | 2018-08-31 | 清华大学 | The device and method for the formaldehyde degradation by photocatalytic oxidation process that bismuth copper sulphur oxygen and/or its composite material and preparation method and purposes, temperature influence |
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| CN108465473A (en) * | 2018-03-13 | 2018-08-31 | 清华大学 | The device and method for the formaldehyde degradation by photocatalytic oxidation process that bismuth copper sulphur oxygen and/or its composite material and preparation method and purposes, temperature influence |
| CN108465473B (en) * | 2018-03-13 | 2021-01-26 | 清华大学 | Bismuth-copper-sulfur oxide and/or composite material thereof, preparation method and application thereof, and equipment and method for photocatalytic degradation of formaldehyde under influence of temperature |
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