CN102120612B - Preparation method of anatase type titanium dioxide nanoparticles - Google Patents
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- CN102120612B CN102120612B CN 201110028522 CN201110028522A CN102120612B CN 102120612 B CN102120612 B CN 102120612B CN 201110028522 CN201110028522 CN 201110028522 CN 201110028522 A CN201110028522 A CN 201110028522A CN 102120612 B CN102120612 B CN 102120612B
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Abstract
The invention relates to a preparation method of anatase type titanium dioxide nanoparticles, comprising the steps of: subjecting a titanium source and inorganic acid to reaction by weight percentage to generate a titanium dispersion solution, making inorganic alkali react with an inorganic salt solution to generate an inorganic alkali dispersion solution, adding a surfactant into the inorganic alkali dispersion solution to generate white precipitates, centrifugally separating, washing and drying to obtain a product. Compared with the prior art, in the invention, the inorganic salt and the inorganic acid are used as dispersing agents, no organic solvent is used in a preparation process, and the preparation method has the advantages of simplicity for material selection and low price, is free of environment pollution and high-temperature roasting, and is beneficial to saving energy, reducing cost and improving economic benefits.
Description
Technical field
The present invention relates to a kind of preparation method of titanium oxide, a kind of specifically method for preparing the anatase titanium dioxide nanoparticle.
Background technology
Titanium oxide is a kind of multi-crystalline compounds harmless to human non-toxic, three kinds of crystal habits is arranged, brookite type, anatase octahedrite and rutile; At present, the nanometer anatase titania particle diameter is even, and good dispersivity, nontoxic has very strong photochemical catalysis, shielding ultraviolet rays ability and the excellent transparency, has been widely used in makeup, the product such as sun-proof as a kind of type material; Nanometer anatase titania has good photochemical catalysis effect, is widely used in photocatalyst and air clearing product.Anatase titanium dioxide is owing to have very strong receptivity to the UV-light in the sunshine simultaneously; And self have very strong reactive behavior and stability, also be applied to aspects such as a lot of technical fields such as fine ceramics, high-grade paint, sun care preparations, photocatalyst, chemical catalysis agent carrier, photochromics; Anatase titanium dioxide nanometer particle process method in the market mainly contains vapor phase process and liquid phase method, vapor phase process and two kinds of method synthesizing anatases of liquid phase method type titanium dioxide nano-particle, and the method complex process requires too high temperature during reaction.The prepared titanium dioxide nano-particle purity of vapor phase process is high, good dispersivity, but its required complex equipments, energy consumption is big, cost is high; Liquid phase method has that facility investment is few, technology is simple, easy to operate, low cost and other advantages; But liquid phase method is divided into the precipitator method, hydrothermal method, microemulsion method and sol-gel method etc. again; Wherein the precipitator method need high-temperature roasting to obtain titanium dioxide nano-particle; High-temperature roasting expends the energy and is prone to reunites, and cost is high, does not belong to low-carbon economy; Hydrothermal method does not need high-temperature roasting, but this method complicated operation, high to equipment requirements is difficult for suitability for industrialized production; Microemulsion method is a kind of method of utilizing two kinds of mutual exclusive solvents synthetic solid phase under influence of surfactant; The tensio-active agent that this method is introduced is difficult for reclaiming, contaminate environment, and influences product purity, does not belong to low-carbon economy equally; Do not meet environmental protection concept; Investment simultaneously is big, and economic benefit is low, and production cost is high.
Summary of the invention
The present invention for address the above problem provide a kind of anatase titanium dioxide nanometer particle process method, this method have that technology is simple, condition simply is easy to control, with low cost, pollution-free, need not pyroprocessing, invest little, with low cost.
The object of the present invention is to provide a kind of anatase titanium dioxide nanometer particle process method, concrete grammar is:
Step 1, get 30-40% titanium source by weight percentage, 60-70% mineral acid mixes, and makes titanium source acid dispersion, and is subsequent use;
Step 2, choose 30-40% sodium hydroxide by weight percentage, 59-65% inorganic salt solution adds sodium hydroxide and makes its dissolving in inorganic salt solution; The back drips 1-5% AS; Stir and end, make mineral alkali alkalescence dispersion liquid, packing is subsequent use;
Step 3, in 60-100 minutes, titanium source acid dispersion is dripped in mineral alkali alkalescence dispersion liquid, can not mineral alkali alkalescence dispersion liquid be joined in the acid dispersion of titanium source, stir; Generate white depositions A, continue to stir 60-70 minutes, after be put in whizzer and separate; Rotating speed is 300 rev/mins, 5-10 minutes time, obtains sediment B and centrifugate A; Centrifugate A reclaims again and utilizes, and sediment B is subsequent use;
Step 4, in 1 part sediment B, add 8-10 times deionized water by ratio of weight and the number of copies; Utilize deionized water to throw out washing 1-3 times, after put into whizzer and separate 400-500 rev/mins of rotating speeds; 5-10 minutes time; Obtain throw out C and centrifugate B, centrifugate B reclaims again and utilizes, and throw out C is subsequent use;
Step 5, in 1 part throw out C, add 8-10 times water-ethanol mixed solution by ratio of weight and the number of copies; Utilize the water-ethanol mixed solution that throw out C is carried out 1-3 washings, after put into whizzer and separate 400-600 rev/mins of rotating speeds; Centrifugation time 5-10 minutes; Obtain sediment D and centrifugate C, centrifugate C reclaims again and utilizes, and sediment D is subsequent use;
Step 6, in 1 part sediment D, add 8-10 times ethanol by ratio of weight and the number of copies, utilize ethanol sediment D washing 1-2 times, after be put in whizzer and separate; 500-1000 rev/mins of rotating speeds, obtain throw out E and centrifugate D at 5-10 minutes time; Centrifugate D is reclaimed; E puts into drying baker with throw out, and drying obtains product.
Described AS is a kind of in sodium lauryl sulphate or the X 2073.
Described mineral acid is a kind of solution in sulfuric acid or the hydrochloric acid, and vitriolic concentration is 98%, and the concentration of hydrochloric acid is 37%.
Described inorganic salt solution is a kind of solution in metabisulfite solution or the sodium chloride solution.
Described titanium source is a kind of in titanium sulfate, titanyl sulfate or the titanium tetrachloride.
Described water-ethanol mixed solution is the mixed solution that the ethanol of 20% water and 80% is formed.
Described titanium oxide is white nanoparticle, is Detitanium-ore-type, crystal grain 3.0-4.0nm, and specific surface area is 1.50 * 10
9/ m-2.00 * 10
9/ m.
Described specific surface area is the surface-area in the unit volume.
Beneficial effect
Must titanium source acid dispersion be added in the mineral alkali alkalescence dispersion liquid among the present invention; Under the situation that does not need high-temperature roasting, hydrolysis to extract; Can anatase titanium dioxide be separated, promptly save energy consumption, reduce environmental pollution again; Reduce production costs, can not get anatase titanium dioxide and mineral alkali alkalescence dispersion liquid is added in the acid dispersion of titanium source.
The present invention compared with prior art; Adopt inorganic salt, mineral acid as dispersion agent, in the preparation process, do not need organic solvent, the selection simple cheap; Cheap; Organic solvent has toxicity mostly or has contaminative, and the inorganic salt of choosing among the present invention, mineral acid environmentally safe do not cause problems such as ecological crisis again.
Can the centrifugate A that reclaim can directly be used for producing as raw material once more in the present invention; The centrifugate B that reclaims can put into the airing pond and make its moisture that volatilizees naturally, utilizes again; Centrifugate C that reclaims and centrifugate D can reclaim ethanol with zero(ppm) water is used for producing again through simple distillation, thereby reduce production costs, the minimizing wasting of resources, increase economic benefit.
The AS that adopts in the technology of the present invention, AS can reduce the reunion of titanium oxide, forms independent small-particle, helps the formation of anatase titania more.
Process method of the present invention is simple, safety, and the inorganic salt of use can reclaim in the process of extracting, and carry out recycling next time; In the process of preparation, do not need high-temperature roasting simultaneously, save the energy, reduce cost; Dispersion agent belongs to the commercially available prod simultaneously, and it is convenient to buy.
Description of drawings
Fig. 1 is an anatase titanium dioxide Raman spectrum collection of illustrative plates of the present invention.
Embodiment
Embodiment 1
Step 1, get 30% titanium sulfate by weight percentage, 70% sulfuric acid mixes, and makes titanium source acid dispersion, and is subsequent use;
Step 2, choose 30% sodium hydroxide by weight percentage, 65% metabisulfite solution adds sodium hydroxide and makes its dissolving in metabisulfite solution, and the sodium lauryl sulphate of back Dropwise 5 % stirs and ends, and makes the alkaline dispersion liquid of mineral alkali, and packing is subsequent use;
Step 3, in 60 minutes, titanium source acid dispersion is dripped in mineral alkali alkalescence dispersion liquid, can not mineral alkali alkalescence dispersion liquid be joined in the acid dispersion of titanium source, stir; Generate white depositions A, continue to stir 60 minutes, after be put in whizzer and separate; Rotating speed is 300 rev/mins, and centrifugation time 5 minutes obtains sediment B and centrifugate A; Centrifugate A reclaims again and utilizes, and sediment B is subsequent use;
Step 4, in 1 part sediment B, add 8 times deionized water by ratio of weight and the number of copies; Utilize deionized water to throw out washing 1 time, after put into whizzer and separate, rotating speed is 400 rev/mins; Centrifugation time 5 minutes; Obtain throw out C and centrifugate B, centrifugate B reclaims again and utilizes, and throw out C is subsequent use;
Step 5, in 1 part throw out C, add 8 times water-ethanol mixed solution by ratio of weight and the number of copies; Utilize the water-ethanol mixed solution that throw out C is carried out 1 time, after put into whizzer and separate, rotating speed is 400 rev/mins; Centrifugation time 5 minutes; Obtain sediment D and centrifugate C, centrifugate C reclaims again and utilizes, and sediment D is subsequent use;
Step 6, in 1 part sediment D, add 8 times ethanol by ratio of weight and the number of copies, utilize ethanol sediment D washing 1 time, after be put in whizzer and separate; Rotating speed is 500 rev/mins, and centrifugation time 5 minutes obtains throw out E and centrifugate D; Centrifugate D is reclaimed, and E puts into drying baker with throw out, drying; Obtain anatase titanium dioxide, its particle diameter is 3.0nm, and specific surface area is 2.00 * 10
9/ m.
Embodiment 2
Step 1, get 40% titanium sulfate by weight percentage, 60% hydrochloric acid mixes, and makes titanium source acid dispersion, and is subsequent use;
Step 2, choose 40% sodium hydroxide by weight percentage, 59% sodium chloride solution adds sodium hydroxide and makes its dissolving in sodium chloride solution, and the back drips 1% X 2073, stirs to end, and makes mineral alkali alkalescence dispersion liquid, and packing is subsequent use;
Step 3, in 70 minutes, titanium source acid dispersion is dripped in mineral alkali alkalescence dispersion liquid, can not mineral alkali alkalescence dispersion liquid be joined in the acid dispersion of titanium source, stir; Generate white depositions A, continue to stir 62 minutes, after be put in whizzer and separate; Rotating speed is 300 rev/mins, 6 minutes time, obtains sediment B and centrifugate A; Centrifugate A reclaims again and utilizes, and sediment B is subsequent use;
Step 4, in 1 part sediment B, add 8 times deionized water by ratio of weight and the number of copies; Utilize deionized water to throw out washing 1 time, after put into whizzer and separate 400 rev/mins of rotating speeds; 6 minutes time; Obtain throw out C and centrifugate B, centrifugate B reclaims again and utilizes, and throw out C is subsequent use;
Step 5, in 1 part throw out C, add 8 times water-ethanol mixed solution by ratio of weight and the number of copies; Utilize the water-ethanol mixed solution that throw out C is carried out 1 washing, after put into whizzer and separate 400 rev/mins of rotating speeds; Centrifugation time 6 minutes; Obtain sediment D and centrifugate C, centrifugate C reclaims again and utilizes, and sediment D is subsequent use;
Step 6, in 1 part sediment D, add 8 times ethanol by ratio of weight and the number of copies, utilize ethanol sediment D washing 1-2 times, after be put in whizzer and separate; 600 rev/mins of rotating speeds, obtain throw out E and centrifugate D at 6 minutes time; Centrifugate D is reclaimed, and E puts into drying baker with throw out, drying; Obtain anatase titanium dioxide, its particle diameter is 3.2nm, and specific surface area is 1.89 * 10
9/ m.
Embodiment 3
Step 1, get 30% titanium tetrachloride by weight percentage, 70% sulfuric acid mixes, and makes titanium source acid dispersion, and is subsequent use;
Step 2, choose 30% sodium hydroxide by weight percentage, 65% metabisulfite solution adds sodium hydroxide and makes its dissolving in metabisulfite solution, and the sodium lauryl sulphate of back Dropwise 5 % stirs and ends, and makes the alkaline dispersion liquid of mineral alkali, and packing is subsequent use;
Step 3, in 70 minutes, titanium source acid dispersion is dripped in mineral alkali alkalescence dispersion liquid, can not mineral alkali alkalescence dispersion liquid be joined in the acid dispersion of titanium source, stir; Generate white depositions A, continue to stir 64 minutes, after be put in whizzer and separate; Rotating speed is 300 rev/mins, 7 minutes time, obtains sediment B and centrifugate A; Centrifugate A reclaims again and utilizes, and sediment B is subsequent use;
Step 4, in 1 part sediment B, add 8 times deionized water by ratio of weight and the number of copies; Utilize deionized water to throw out washing 1 time, after put into whizzer and separate 400 rev/mins of rotating speeds; 7 minutes time; Obtain throw out C and centrifugate B, centrifugate B reclaims again and utilizes, and throw out C is subsequent use;
Step 5, in 1 part throw out C, add 9 times water-ethanol mixed solution by ratio of weight and the number of copies; Utilize the water-ethanol mixed solution that throw out C is carried out 2 washings, after put into whizzer and separate 500 rev/mins of rotating speeds; Centrifugation time 7 minutes; Obtain sediment D and centrifugate C, centrifugate C reclaims again and utilizes, and sediment D is subsequent use;
Step 6, in 1 part sediment D, add 9 times ethanol by ratio of weight and the number of copies, utilize ethanol sediment D washing 1 time, after be put in whizzer and separate; 700 rev/mins of rotating speeds, obtain throw out E and centrifugate D at 7 minutes time; Centrifugate D is reclaimed, and E puts into drying baker with throw out, drying; Obtain anatase titanium dioxide, its particle diameter is 3.5nm, and specific surface area is 1.71 * 10
9/ m.
Embodiment 4
Step 1, get 40% titanium tetrachloride by weight percentage, 60% hydrochloric acid mixes, and makes titanium source acid dispersion, and is subsequent use;
Step 2, choose 40% sodium hydroxide by weight percentage, 59% sodium chloride solution adds sodium hydroxide and makes its dissolving in sodium chloride solution, and the back drips 1% X 2073, stirs to end, and makes mineral alkali alkalescence dispersion liquid, and packing is subsequent use;
Step 3, in 80 minutes, titanium source acid dispersion is dripped in mineral alkali alkalescence dispersion liquid, can not mineral alkali alkalescence dispersion liquid be joined in the acid dispersion of titanium source, stir; Generate white depositions A, continue to stir 66 minutes, after be put in whizzer and separate; Rotating speed is 300 rev/mins, 8 minutes time, obtains sediment B and centrifugate A; Centrifugate A reclaims again and utilizes, and sediment B is subsequent use;
Step 4, in 1 part sediment B, add 9 times deionized water by ratio of weight and the number of copies; Utilize deionized water to throw out washing 2 times, after put into whizzer and separate 500 rev/mins of rotating speeds; 8 minutes time; Obtain throw out C and centrifugate B, centrifugate B reclaims again and utilizes, and throw out C is subsequent use;
Step 5, in 1 part throw out C, add 9 times water-ethanol mixed solution by ratio of weight and the number of copies; Utilize the water-ethanol mixed solution that throw out C is carried out 2 washings, after put into whizzer and separate 600 rev/mins of rotating speeds; Centrifugation time 8 minutes; Obtain sediment D and centrifugate C, centrifugate C reclaims again and utilizes, and sediment D is subsequent use;
Step 6, in 1 part sediment D, add 9 times ethanol by ratio of weight and the number of copies, utilize ethanol sediment D washing 2 times, after be put in whizzer and separate; 800 rev/mins of rotating speeds, obtain throw out E and centrifugate D at 8 minutes time; Centrifugate D is reclaimed, and E puts into drying baker with throw out, drying; Obtain anatase titanium dioxide, its particle diameter is 3.7nm, and specific surface area is 1.62 * 10
9/ m.
Embodiment 5
Step 1, get 30% titanyl sulfate by weight percentage, 70% sulfuric acid mixes, and makes titanium source acid dispersion, and is subsequent use;
Step 2, choose 30% sodium hydroxide by weight percentage, 65% metabisulfite solution adds sodium hydroxide and makes its dissolving in metabisulfite solution, and the sodium lauryl sulphate of back Dropwise 5 % stirs and ends, and makes the alkaline dispersion liquid of mineral alkali, and packing is subsequent use;
Step 3, in 90 minutes, titanium source acid dispersion is dripped in mineral alkali alkalescence dispersion liquid, can not mineral alkali alkalescence dispersion liquid be joined in the acid dispersion of titanium source, stir; Generate white depositions A, continue to stir 68 minutes, after be put in whizzer and separate; Rotating speed is 300 rev/mins, 9 minutes time, obtains sediment B and centrifugate A; Centrifugate A reclaims again and utilizes, and sediment B is subsequent use;
Step 4, in 1 part sediment B, add 10 times deionized water by ratio of weight and the number of copies; Utilize deionized water to throw out washing 3 times, after put into whizzer and separate 500 rev/mins of rotating speeds; 9 minutes time; Obtain throw out C and centrifugate B, centrifugate B reclaims again and utilizes, and throw out C is subsequent use;
Step 5, in 1 part throw out C, add 10 times water-ethanol mixed solution by ratio of weight and the number of copies; Utilize the water-ethanol mixed solution that throw out C is carried out 3 washings, after put into whizzer and separate 600 rev/mins of rotating speeds; Centrifugation time 9 minutes; Obtain sediment D and centrifugate C, centrifugate C reclaims again and utilizes, and sediment D is subsequent use;
Step 6, in 1 part sediment D, add 10 times ethanol by ratio of weight and the number of copies, utilize ethanol sediment D washing 2 times, after be put in whizzer and separate; 900 rev/mins of rotating speeds, obtain throw out E and centrifugate D at 9 minutes time; Centrifugate D is reclaimed, and E puts into drying baker with throw out, drying; Obtain anatase titanium dioxide, its particle diameter is 3.8nm, and specific surface area is 1.58 * 10
9/ m.
Embodiment 6
Step 1, get 40% titanyl sulfate by weight percentage, 60% hydrochloric acid mixes, and makes titanium source acid dispersion, and is subsequent use;
Step 2, choose 40% sodium hydroxide by weight percentage, 59% sodium chloride solution adds sodium hydroxide and makes its dissolving in sodium chloride solution, and the back drips 1% X 2073, stirs to end, and makes mineral alkali alkalescence dispersion liquid, and packing is subsequent use;
Step 3, in 100 minutes, titanium source acid dispersion is dripped in mineral alkali alkalescence dispersion liquid, can not mineral alkali alkalescence dispersion liquid be joined in the acid dispersion of titanium source, stir; Generate white depositions A, continue to stir 70 minutes, after be put in whizzer and separate; Rotating speed is 300 rev/mins, 10 minutes time, obtains sediment B and centrifugate A; Centrifugate A reclaims again and utilizes, and sediment B is subsequent use;
Step 4, in 1 part sediment B, add 10 times deionized water by ratio of weight and the number of copies; Utilize deionized water to throw out washing 3 times, after put into whizzer and separate 500 rev/mins of rotating speeds; 10 minutes time; Obtain throw out C and centrifugate B, centrifugate B reclaims again and utilizes, and throw out C is subsequent use;
Step 5, in 1 part throw out C, add 10 times water-ethanol mixed solution by ratio of weight and the number of copies; Utilize the water-ethanol mixed solution that throw out C is carried out 3 washings, after put into whizzer and separate 600 rev/mins of rotating speeds; Centrifugation time 10 minutes; Obtain sediment D and centrifugate C, centrifugate C reclaims again and utilizes, and sediment D is subsequent use;
Step 6, in 1 part sediment D, add 10 times ethanol by ratio of weight and the number of copies, utilize ethanol sediment D washing 2 times, after be put in whizzer and separate; 1000 rev/mins of rotating speeds, obtain throw out E and centrifugate D at 10 minutes time; Centrifugate D is reclaimed, and E puts into drying baker with throw out, drying; Obtain anatase titanium dioxide, its particle diameter is 4.0nm, and specific surface area is 1.50 * 10
9/ m.
Claims (2)
1. anatase titanium dioxide nanometer particle process method, described titanium oxide is white nanoparticle, is Detitanium-ore-type, crystal grain 3.0-4.0nm, specific surface area is 1.50 * 10
9/ m-2.00 * 10
9/ m is characterized in that: the preparation method is following:
Step 1, get 30-40% titanium source by weight percentage, 60-70% mineral acid mixes, and makes titanium source acid dispersion, and is subsequent use;
Step 2, choose 30-40% sodium hydroxide by weight percentage, 59-65% inorganic salt solution adds sodium hydroxide and makes its dissolving in inorganic salt solution; The back drips 1-5% AS; Stir and end, make mineral alkali alkalescence dispersion liquid, packing is subsequent use; Described AS is an X 2073;
Step 3, in 60-100 minutes, titanium source acid dispersion is dripped in mineral alkali alkalescence dispersion liquid, can not mineral alkali alkalescence dispersion liquid be joined in the acid dispersion of titanium source, stir; Generate white depositions A, continue to stir 60-70 minutes, after be put in whizzer and separate; Rotating speed is 300 rev/mins, 5-10 minutes time, obtains sediment B and centrifugate A; Centrifugate A reclaims again and utilizes, and sediment B is subsequent use;
Step 4, in 1 part sediment B, add 8-10 times deionized water by ratio of weight and the number of copies; Utilize deionized water to throw out washing 1-3 times, after put into whizzer and separate 400-500 rev/mins of rotating speeds; 5-10 minutes time; Obtain throw out C and centrifugate B, centrifugate B reclaims again and utilizes, and throw out C is subsequent use;
Step 5, in 1 part throw out C, add 8-10 times water-ethanol mixed solution by ratio of weight and the number of copies; Utilize the water-ethanol mixed solution that throw out C is carried out 1-3 washings, after put into whizzer and separate 400-600 rev/mins of rotating speeds; Centrifugation time 5-10 minutes; Obtain sediment D and centrifugate C, centrifugate C reclaims again and utilizes, and sediment D is subsequent use;
Step 6, in 1 part sediment D, add 8-10 times ethanol by ratio of weight and the number of copies, utilize ethanol sediment D washing 1-2 times, after be put in whizzer and separate; 500-1000 rev/mins of rotating speeds, obtain throw out E and centrifugate D at 5-10 minutes time; Centrifugate D is reclaimed; E puts into drying baker with throw out, and drying obtains product;
Described mineral acid is a kind of solution in sulfuric acid or the hydrochloric acid, and vitriolic concentration is 98%, and the concentration of hydrochloric acid is 37%;
Described inorganic salt solution is a kind of solution in metabisulfite solution or the sodium chloride solution;
Described titanium source is a kind of in titanium sulfate, titanyl sulfate or the titanium tetrachloride.
2. a kind of anatase titanium dioxide nanometer particle process method according to claim 1 is characterized in that: described water-ethanol mixed solution is the mixed solution that the ethanol of 20% water and 80% is formed.
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| Title |
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| 符崖 等.表面活性剂对溶胶凝胶法制备TiO2纳米晶的影响.《医疗卫生装备》.2005,第26卷(第8期),第25、28页. * |
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