Photocatalyst powder and preparation method thereof

A kind of photocatalyst powder and its preparation method

Technical field

[0001] The present invention relates to the technical field of chemical products, and more particularly to a photocatalyst powder and a process for its preparation.

Background technique

[0002] Photocatalyst (photo + catalyst (catalyst) synthesis word), is a nano-metal oxide material, under the action of light, it can air or oxygen in the air catalytic oxidation capacity of the strong hydroxyl Free radicals (· 0H), superoxide anion radicals (O2), active oxygen (HO2, H2O2), and the like. The energy of these reactive groups is equivalent to the high temperature of 3600K, Strong oxidizing, they are in contact with the surrounding harmful gases, contaminants, bacteria contact, the redox reaction. These strong oxidizing groups can effectively decompose all kinds of organic compounds with unstable chemical bonds and some inorganic substances, and can destroy the bacterial cell membrane and coagulation virus protein carrier, with a strong sterilization, deodorant, anti-pollution self-cleaning , Purify the air function, so as to achieve the purification of the environment, the function of air purification.

[0003] Simple photocatalyst powder in the form of powder, easy to blow off the wind, not practical, it must be made of adhesive type solution (usually refers to the paint). When the adhesive solution containing the photocatalyst powder is sprayed onto the target (e.g., furniture), it is dried and adsorbed on the target, which is not easily worn and dropped.

[0004] However, the use of existing photocatalyst powder prepared from the paint, there is generally poor weather resistance, poor adhesion of the shortcomings.

The contents of the invention

In order to overcome the shortcomings of the prior art, it is a first object of the present invention to provide a photocatalyst powder which is simple in composition, has excellent catalytic and oxidative ability, is capable of efficiently decomposing toxic substances, has high purification efficiency and good weather resistance.

[0006] A second object of the present invention is to provide a method for producing a photocatalyst powder which is simple in steps, simple in process, operable and low in preparation cost.

[0007] The first object of the present invention is achieved by the following technical scheme:

[008] The photoconductive powder is prepared from the following components in weight percent: 35-65% of metatitanic acid; 0.5 to 2.5% of composition A;

[0009] Alkaline oxide solution 1-10%; Titanium Sulfate Balance ί

Wherein the composition A is composed of a mixture of a metal oxide and a non-metal oxide in any ratio.

[0011] Preferably, the metal oxide is chromium oxide; the non-metallic oxide is silica; and the alkaline oxide solution is a sodium hydroxide solution.

[0012] Preferably, the concentration of the alkaline oxide solution is 1.2 to 1.35 mol / L.

[0013] is preferably prepared from the following components in weight percent: metatitanic acid 45-55%; composition A 1-2%

[0014] Alkaline oxide solution 3-H%, titanyl sulfate scale;

Wherein the composition A is mixed with a metal oxide and a non-metal oxide in any ratio.

[0016] is preferably prepared from the following components in weight percent: metatitanic acid 50%; metal oxide l ° Zo: 5

[0017] Non-metallic oxide 1%; Alkaline oxide solution 5%; Titanium sulfate 43%.

[0018] is preferably prepared from the following components by weight: 50% of metatitanic acid; 0.5% metal oxide;

[0019] Non-metallic oxide 0.5%; Alkaline oxide solution 5%; Titanium sulfate 44%.

[0020] is preferably prepared from the following components in weight percent: metatitanic acid 45%; metal oxide 0.1%;

[0021] non-metallic oxide 2%; alkaline oxide solution 8%, titanium sulfate 45.7%.

[0022] is preferably prepared from the following components in weight percent:

[0023] 55% of metatitanic acid; 1.5% of metal oxide; 0.1% of non-metallic oxide;

[0024] Alkaline oxide solution 3% ;: 40.4% of titanyl sulfate.

[0025] The second object of the present invention is achieved by the following technical scheme:

[0026] The preparation process of the photocatalyst powder comprises the following steps:

[0027] 1) The formulation amount of titanyl titanate, metatitanic acid and composition A were put into a stirrer and stirred uniformly to obtain a first mixture;

2) mixing the formulated amount of the alkaline oxide solution into the agitator, mixing with the first mixture and stirring for 8-12 min to obtain a second mixture, the second mixture being a solid-liquid mixture;

[0029] 3) The second mixture is subjected to solid-liquid separation to obtain a solid mixture and a liquid mixture;

[0030] 4) The solid mixture is dried and dried in an environment of 100-150 ° c or less to obtain a first semi-finished product;

[0031] 5) calcining the first semi-finished product to obtain a second semi-finished product;

[0032] 6) The second semi-finished product is ground to obtain the photocatalyst powder.

[0033] That is, the photocatalyst powder is subjected to a liquid phase precipitation method, and then subjected to low temperature drying, controlled temperature calcination, and sanding.

[0034] Preferably, in step 1), the agitator has a rotational speed of 1200 r / min and a stirring time of 25-35 min; in step 2), the stirring time is IOmin; in step 4), the drying time is 0.7 -1.2h; in step 5), the calcination temperature is 1200-1300 ° C and the calcination time is 4.5-5.5h; in step 6), the second semi-finished product is fed into a nano-sand mill, 5 times, wherein the main motor power of the nano-sand mill is 11 kW and the rotational speed is 2000 r / min.

[0035] The advantageous effect of the present invention over the prior art is that,

(1) The photocatalyst powder provided by the present invention can catalyze the water or oxygen in the air to a hydroxyl radical (· 0H), a superoxide anion radical (O2 ·), an active oxygen (HO2 ·, H2O2) and other strong oxidizing ability of the active group, play a good sterilization, deodorant, anti-fouling self-cleaning, the role of air purification, thus purifying the environment, purify the air.

(2) The photocatalyst powder, the metal oxide and the non-metallic oxide provided by the present invention play an important role, and when the weight percentage thereof is in the range of 1 to 2%, the photocatalytic effect of the photocatalyst powder is best The

(3) The photocatalyst powder provided by the present invention is suitable for preparing a coating material, and the prepared paint is not easily worn and dropped, has good weather resistance, has strong adhesion, and more importantly, it can greatly increase the negative ions in the air The concentration of clean air, fresh air pleasant, is conducive to good health.

(4) The method for preparing the photocatalyst powder provided by the present invention is carried out in a step of 4) in an environment of 100 to 150 ° C, exceeding 150 ° C, which reduces the silica activity and low At 100 ° C, moisture is difficult to evaporate and can not dry.

detailed description

[0040] Hereinafter, the present invention will be described in further detail with reference to specific embodiments thereof:

[0041] A photocatalyst powder prepared from the following components in weight percent: 35-65% of metatitanic acid; composition A 0.5-2.5%

[0042] Alkaline oxide solution 1-10% Sulfuric acid Oxygen balance;

Wherein the composition A is mixed with a metal oxide and a non-metal oxide in any ratio.

[0044] As a preferred embodiment, the metal oxide is chromium oxide; the non-metallic oxide is silica; the alkaline oxide solution is a sodium hydroxide solution at a concentration of 1.2-1.35 mol / L The

[0045] As a preferred embodiment, prepared from the following components in weight percent: meta-titanic acid 45-55% Composition A 1-2%

[0046] Alkaline oxide solution 3-8%; titanyl sulfate;

Wherein the composition A is mixed with a metal oxide and a non-metal oxide in any ratio. Metal oxides and non-metallic oxides play an important role, when their weight percentage of 1-2%, the catalytic oxidation effect to achieve the best.

[0048] A process for preparing a photocatalyst powder comprising the steps of:

[0049] 1) The formulation amount of titanyl titanate, metatitanic acid and composition A were put into a stirrer and stirred uniformly to obtain a first mixture;

2) mixing the formulated amount of the alkaline oxide solution into the agitator, mixing with the first mixture and stirring for 8-12 min to obtain a second mixture, the second mixture being a solid-liquid mixture;

[0051] 3) The second mixture is subjected to solid-liquid separation to obtain a solid mixture and a liquid mixture;

[0052] 4) The solid mixture is dried and dried in an environment of 100 to 150 ° C to obtain a first semi-finished product;

[0053] 5) calcining the first semi-finished product to obtain a second semi-finished product;

[0054] 6) The second semi-finished product is ground to obtain the photocatalyst powder.

In step 1), the stirring speed of the agitator is 1200r / min and the stirring time is 25-35min; in step 2), the stirring time is IOmin; in step 4), the drying time Is in the range of 0.7 to 1.2 h; in step 5), the calcination temperature is 1200-1300 ° C and the calcination time is 4.5-5.5 h; in step 6), the second semi-finished product is fed into a nano-sand mill, 3-5 times, wherein the main motor power of the nano-sand mill is 11KW and the rotational speed is 2000r / min.

[0056] Example 1

The photocatalyst powder is prepared from metatitanic acid, composition A (metal oxide and non-metal oxide), alkaline oxide solution and titanyl sulfate, and the weight percentage of each of the components is shown in Table 1. The photocatalyst powder was prepared according to the following procedure:

[0058] 1) The formula amount of titanyl titanate, metatitanic acid and composition A were put into a stirrer, the stirring speed was set to 1200r / min, the stirring time was 30min, and the first mixture was obtained after stirring.

[0059] 2) mixing the formulated amount of the alkaline oxide solution into the agitator, mixing with the first mixture and stirring the IOmin to obtain a second mixture, the second mixture being a solid-liquid mixture;

[0060] 3) The second mixture is subjected to solid-liquid separation to obtain a solid mixture and a liquid mixture;

[0061] 4) The solid mixture was dried and left in an environment of 150 ° C or less to obtain a first semi-finished product;

[0062] 5) The first semi-finished product was placed in an environment of 1250? For 5 hours to obtain a second semi-finished product;

6) The second semi-finished product was put into a nano-sand mill and circulated for 4 times, wherein the main motor power of the nano-sand mill was 11 kW and the rotational speed was 2000 r / min to obtain the photocatalyst powder.

[0064] Example 2

The photocatalyst powder is prepared from metatitanic acid, composition A (metal oxide and non-metal oxide), alkaline oxide solution and titanyl sulfate, and the weight percentage of each of the components is shown in Table 1. The photocatalyst powder was prepared according to the following procedure:

[0066] 1) The formula amount of titanyl titanate, meta-titanic acid and composition A were put into a stirrer, the stirring speed was set to 1200r / min, the stirring time was 25min, and the first mixture was obtained after stirring.

2) mixing the formulated amount of the basic oxide solution into the agitator, mixing with the first mixture and stirring for 12 minutes to obtain a second mixture, the second mixture being a solid-liquid mixture;

[0068] 3) The second mixture is subjected to solid-liquid separation to obtain a solid mixture and a liquid mixture;

[0069] 4) The solid mixture was placed in an environment of 150 ° C or less and dried for 0.7 h to obtain a first semi-finished product;

[0070] 5) The first semi-finished product was calcined at 1200 ° C for 5.5 h to obtain a second semi-finished product;

6) The second semi-finished product was put into a nano-sand mill and circulated for 3 times, wherein the main motor power of the nano-sand mill was 11 kW and the rotational speed was 2000 r / min to obtain the photocatalyst powder.

[0072] Example 3

The photocatalyst powder is prepared from metatitanic acid, composition A (metal oxide and non-metal oxide), alkaline oxide solution and titanyl sulfate, and the weight percentage of each of the components is shown in Table 1. The photocatalyst powder was prepared according to the following procedure:

1) The formulation amount of titanyl titanate, metatitanic acid and composition A were put into a stirrer, the stirring speed of the mixer was set to 1200r / min, the stirring time was 35min, and the first mixture was obtained after stirring.

2) mixing the formulated amount of the alkaline oxide solution into the agitator, mixing with the first mixture and stirring Smin to obtain a second mixture, the second mixture being a solid-liquid mixture;

[0076] 3) The second mixture is subjected to solid-liquid separation to obtain a solid mixture and a liquid mixture;

[0077] 4) The solid mixture was placed in an environment of 150 ° C or less and dried for 1.2 hours to obtain a first semi-finished product;

[0078] 5) The first semi-finished product was calcined at 1300 ° C for 4.5 hours to obtain a second semi-finished product;

6) The second semi-finished product was put into a nano-sand mill and circulated for 5 times, wherein the main motor power of the nano-sand mill was 11 kW and the rotational speed was 2000 r / min to obtain the photocatalyst powder.

[0080] Example 4

The photocatalyst powder is prepared from meta-titanic acid, composition A (metal oxide and non-metal oxide), alkaline oxide solution and titanyl sulfate, and the weight percentage of each of the components is shown in Table 1. The photocatalyst powder was prepared according to the following procedure:

[0082] 1) The formulation amount of titanyl sulfate, metatitanic acid and composition A were put into a stirrer, the stirring speed of the mixer was set to 1200r / min, the stirring time was 32min, and the first mixture was obtained after stirring.

2) mixing the formulated amount of the alkaline oxide solution into the agitator, mixing with the first mixture and stirring I Imin to obtain a second mixture, the second mixture being a solid-liquid mixture;

[0084] 3) The second mixture is subjected to solid-liquid separation to obtain a solid mixture and a liquid mixture;

[0085] 4) The solid mixture was placed in an environment of 150 ° C or less and dried for 0.9 h to obtain a first semi-finished product;

[0086] 5) The first semi-finished product was calcined at 1280 ° C for 4.8 h to obtain a second semi-finished product;

6) The second semi-finished product was put into a nano-sand mill and circulated for 4 times, wherein the main motor power of the nano-sand mill was 11 kW and the rotational speed was 2000 r / min to obtain the photocatalyst powder.

[0088] Example 5

[0089] Example 5 differs from Example 1 in that the weight percentage of Composition A is 0.5% and the weight percentage of titanyl sulfate is 44.5%.

[0090] Example 6

[0091] Example 6 differs from Example 2 in that the weight percentage of Composition A is 0.9% and the weight percentage of titanyl sulfate is 44.1%.

[0092] Example 7

[0093] Example 7 differs from Example 3 in that the weight percentage of Composition A is 2.5% and the weight percentage of titanyl sulfate is 44.5%.

[0094] Comparative Example 1

[0095] Comparative Example 1 differs from Example 1 in that the weight percentage of the composition A is 0.1% and the weight percentage of the titanyl sulfate is 44.9%.

[0096] Comparative Example 2

[0097] Comparative Example 2 differs from Example 2 in that the weight percentage of Composition A is 0.4% and the weight percentage of titanyl sulfate is 44.6%.

[0098] Comparative Example 3

[0099] Comparative Example 3 differs from Example 3 in that the weight percentage of Composition A is 3% and the weight percentage of titanyl sulfate is 44%.

[0100] Table 1 Formulation of photocatalyst powder of Example 1 -7 and Comparative Example 1 -3

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[0102] Test example

In order to verify the air purifying ability of the photocatalyst powder obtained in Examples 1 to 7 and Comparative Examples 1 to 3, the photocatalyst powder of Examples 1 to 7 and Comparative Examples 1 to 3 was prepared and subjected to coating 10 different coatings. The specific composition of the prepared coating is as follows:

[0104] Photocatalyst powder 13%; nano-silica 20%; modified fluorocarbon resin 1%; defoamer 0.1%; coupling agent 0.1%; to Shangzi water, the balance.

[0105] Test method: The samples of Examples 1 to 7 and the coatings of Comparative Examples 1 to 3 were prepared, and five samples were prepared for each of the coatings. The samples were prepared as follows: 50 cm x 50 cmX 2cm clean wood board, in its surface evenly coated with thickness of 1-0.3cm of paint, until the paint is dry. Five samples of each coating were placed in a 20m3 sample compartment. After 24 hours, the concentration of negative ions in the sample compartment was measured by air ion measuring instrument. The test results are shown in Table 2 below.

[0106] Negative ion concentration refers to the number of negative ions per unit volume of air, according to the United Nations Health Organization standards, the air anion content of 1500 / cm3, is the standard of fresh air; to 2.0 X IO4 / cm3 above, then Has the effect of health care.

[0107] Table 2 Example 1 -7 and Comparative Example 1 -3 Photocatalyst Coatings Negative Ion Release Capability Record Table

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As shown in Table 2, the negative ion releasing ability of the nanometer photocatalyst coating obtained in Examples 1 to 7 was excellent in purifying the air, and particularly, the coatings of Examples 1 to 4, The weight percent of the metal oxide and the non-metal oxide in the photocatalyst powder is within 1 to 2%, and the concentration of the negative ions in the sample compartment is in the range of 3.OX IO3 / cm3 or more, particularly in Example 1 Sample cabin, anion concentration of 4.OX IO3 / cm3, fresh air, the paint the best cleaning effect.

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In the coatings of Examples 5 to 7, the weight percentages of the metal oxides and the non-metallic oxides in the photocatalyst powder were 0.5%, 0.9% and 2.5%, respectively, and the negative ion concentrations were 2.8 X IO3 / Cm3, 3.0 X IO3 / cm3, 2.7 X IO3 / cm3, both lower than the sample compartments of Examples 1-4, the air is fresh and the coating is better.

In the coatings of Comparative Examples 1-3, the percentages of metal oxides and non-metallic oxides in the photocatalyst powder were 0.1%, 0. 4% and 3%, respectively, and the corresponding negative ion concentration was 2.1 X IO3 / cm3, 2.5 X IO3 / cm3 and 2.2 X IO3 / cm3, air freshenity is less than those of Examples 1 to 7, Comparative Examples 1-3 of the nano photocatalyst coating negative ion release capacity is relatively poor, Air purification effect is poor.

[0112] Various other changes and modifications may be made to those skilled in the art in light of the technical solutions and concepts described above, and all such changes and modifications are intended to be within the scope of the claims of the claims of the invention Inside.