CN105314674A - Preparation method of ultrasmall nanometer titanium dioxide hybrid material - Google Patents
Preparation method of ultrasmall nanometer titanium dioxide hybrid material Download PDFInfo
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention discloses a preparation method of an ultrasmall nanometer titanium dioxide hybrid material. The method includes the steps that thermoset bifunctional acrylic ester unsaturated resin monomers are used as a solvent system for replacing traditional solvent, a titanium source is dissolved in the solvent, blocky solid containing titanium dioxide precursors is obtained by solidifying unsaturated resin, blocky solid is sintered at a high temperature under the inertia atmosphere after being smashed, and the ultrasmall nanometer titanium dioxide hybrid material is obtained by effectively controlling the appearance of the titanium dioxide nanometer particles when the thermoset resin is difficult to melt in the high-temperature sintering process. By means of the method, acrylic ester unsaturated resin is used as the non-traditional solvent system for preparing the ultrasmall nanometer titanium dioxide hybrid material, and the titanium dioxide nanometer particles with the size smaller than 5 nm and even being 1 nm can be obtained and can be evenly dispersed in a carbon matrix.
Description
Technical field
The present invention relates to a kind of preparation method of nano titanium dioxide hybrid material, especially a kind of method adopting non-traditional solvent system to prepare extra granular nano titanium dioxide hybrid material.
Background technology
Nano titanium oxide has outstanding photoelectric properties, and specific surface area is much larger than ordinary titanium dioxide.Be with a wide range of applications in fields such as coating, wrapping material, makeup, optics, electricity, photochemical catalysis.
The method preparing nano TiO 2 powder seeing report at present is mainly prepared by being hydrolyzed in a solvent in titanium source.The patent No. be 201410211716.6 Chinese patent disclose a kind of preparation method of flower-shaped poriferous titanium dioxide nano material, titanium source is dissolved in deionized water, with urea reaction, product is centrifugal, washing, dry, the steps such as air atmosphere calcining obtain flower-shaped poriferous titanium dioxide nano material.The patent No. is the preparation method that the Chinese patent of CN1418820.A discloses a kind of chrysanthemum flower type nano TiO 2 powder material.Take titanyl sulfate as main raw material, after alkali precipitation washing, be converted into titanyl nitrate, add ordinary-pressure hydrolysis after additive, be separated, washing, drying obtain chrysanthemum flower type titanium dioxide powder material.This method relates to loaded down with trivial details precipitation, separation and washing process, produces a large amount of waste liquid, big for environment pollution and can not amplify production.
Although above method has prepared the titanic oxide material of Nano grade, but preparation process complicated and time consumption, relate to a large amount of organic solvent, to environment, solvent treatment is loaded down with trivial details and expensive, and nano-powder easily produces reunion in the process of dry solvent, there is certain defect, preparation-obtained particle size is comparatively large, and easily reunites.
Summary of the invention
Object of the present invention is exactly for the deficiencies in the prior art, provides a kind of preparation method of simple controlled extra granular nano titanium dioxide hybrid material.
The present invention to the effect that adopts thermoset bifunctional acrylate class unsaturated polyester monomer to replace conventional solvent as solvent system, titanium source is dissolved in this solvent, pass through curing unsaturated resins, obtain the blocks of solid containing TiO 2 precursor, inert atmosphere high-temperature calcination after pulverizing, because thermosetting resin is difficult to melting occurs in high-temperature burning process, so can effectively control titanium dioxide nano-particle pattern, thus obtain extra small nano titania hybrid material.
The concrete steps of the inventive method are:
Step (1). esters of acrylic acid unsaturated polyester monomer and light trigger are uniformly mixed at 60 ~ 80 DEG C, obtain mixed solution; In mixed solution, the mass content of light trigger is 0.2 ~ 2.0 ﹪;
Described esters of acrylic acid unsaturated polyester monomer is one or more in dihydroxyphenyl propane-glycidyl Methacrylate, triethylene glycolbismethyl-acrylate, dimethacrylate glycol ether ester, Ethylene glycol dimethacrylate, TEG dimethacrylate, HDDMA, ethoxylated bisphenol dimethacrylate;
Described light trigger be gorgeous good solid 1173, gorgeous good solid 184, gorgeous good solid 2959, gorgeous good solid 907, gorgeous good solid 369, gorgeous good solid 819, gorgeous good solid 754 or camphorquinone in one or several;
Step (2). titanium source is joined in above-mentioned mixed solution, stir 5 ~ 10 minutes, obtain the mixing solutions containing TiO 2 precursor; Every 10 grams contain 0.001 ~ 5 gram of titanium source containing in the mixing solutions of TiO 2 precursor;
Described titanium source is one or several in Butyl Phthalate, titanium isopropylate, titanyl sulfate, titanium tetrachloride;
Step (3). be injected in mould by the above-mentioned mixing solutions containing TiO 2 precursor, adopt blue light or ultraviolet light polymerization, illumination 60 ~ 240 seconds under 5 ~ 50W power, obtains TiO 2 precursor/polyacrylic ester composite solid material;
Step (5). TiO 2 precursor/polyacrylic ester composite solid material is pulverized, pulverizes 1 ~ 5 minute, obtain solid particulate.
Step (6). by above-mentioned solid particulate at 500 ~ 800 DEG C, calcine 2 ~ 6 hours under inert atmosphere, obtain extra granular nano titanium dioxide hybrid material.
As preferably, inert atmosphere is N
2or argon gas.
The inventive method adopts acrylics unsaturated polyester to prepare extra small nano titania hybrid material as the non-traditional solvent system of one, the titanium dioxide nano-particle that size is less than 5nm (or even 1nm) can be obtained, and can be dispersed in carbon.This inventive method does not use conventional organic solvents, avoids solvent treatment, preparation method's environmental friendliness, and technique simple and fast, condition is controlled.
Accompanying drawing explanation
Fig. 1 is the nano-titanium dioxide powder scanning electron microscope (SEM) photograph of preparation in comparative example 1, and wherein a is high magnification shooting, and b is low range shooting;
Fig. 2 is the nano titanium dioxide hybrid material transmission electron microscope picture of preparation in embodiment 1, and wherein a is microscopic appearance, and b is high resolution.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further analyzed.
Comparative example 1
Step (1). by 4 grams of dihydroxyphenyl propane-glycidyl Methacrylates, 6 grams of triethylene glycolbismethyl-acrylates, be uniformly mixed at 60 DEG C for 0.05 gram gorgeous good solid 819, obtain the mixed solution of 10.05 grams;
Step (2). 3 grams of pluronic F127 are joined in above-mentioned mixed solution, is uniformly mixed at 50 DEG C, form homogeneous 13.05g template solution;
Step (3). 2.5 grams of titanium isopropylates and 0.5 gram of concentrated hydrochloric acid are joined in above-mentioned template solution, stirs 10 minutes, obtain the mixing solutions containing TiO 2 precursor;
Step (4). the mixing solutions containing TiO 2 precursor is injected in mould, adopts the solidification in 60 seconds of 50W blue light illumination, obtain TiO 2 precursor/polyacrylic ester composite solid material;
Step (5). TiO 2 precursor/polyacrylic ester composite solid material is pulverized 1 minute, obtained solid particulate.
Step (6). above-mentioned solid particulate is calcined 4 hours under 800 DEG C of air atmospheres, obtains nano-titanium dioxide powder.
As shown in Figure 1, nano-titanium dioxide powder material particle size prepared by embodiment 1 is about 50nm, and the aperture between nanoparticle is about 50nm, and nanoparticle is gathered into the fluffy block of micron level.
Comparative example 2 ~ 9
Esters of acrylic acid unsaturated polyester monomeric bisphenol A-glycidyl Methacrylate in comparative example 1, triethylene glycolbismethyl-acrylate are replaced by other, and calcination condition adjusts a little, and all the other conditions are constant, specifically in table 1.
Embodiment 1
Step (1). by 4 grams of dihydroxyphenyl propane-glycidyl Methacrylates, 6 grams of triethylene glycolbismethyl-acrylates, be uniformly mixed at 60 DEG C for 0.05 gram gorgeous good solid 819, obtain the mixed solution of 10.05 grams;
Step (2). 0.001 gram of titanium isopropylate is joined in above-mentioned 10.05g mixed solution, stir 10 minutes, obtain the mixing solutions that 10.051g contains TiO 2 precursor;
Step (4). the mixing solutions containing TiO 2 precursor is injected in mould, adopts the solidification in 60 seconds of 50W blue light illumination, obtain TiO 2 precursor/polyacrylic ester composite solid material;
Step (5). TiO 2 precursor/polyacrylic ester composite solid material is pulverized 1 minute, obtained solid particulate.
Step (6). by above-mentioned solid particulate at 800 DEG C of N
2calcine 4 hours under inert atmosphere, obtain nanometer titanium dioxide titanium block material.
As seen from Figure 1, Figure 2, nano-titanium dioxide powder material particle size prepared by embodiment 1 is about 1 nanometer, and nanoparticle is coated by carbon, is dispersed in carbon, and nanoparticle and carbon form other block materials of submicron order.
Embodiment 2
Step (1). 9.98g dihydroxyphenyl propane-glycidyl Methacrylate, 0.02g gorgeous good solid 1173 are uniformly mixed at 80 DEG C, obtain 10g mixed solution;
Step (2). 3g titanium isopropylate is joined in above-mentioned 10g mixed solution, stir 10 minutes, obtain 13g TiO 2 precursor solution;
Step (3). above-mentioned TiO 2 precursor solution is injected in mould, adopts the solidification in 120 seconds of 5W UV Light, obtain TiO 2 precursor/polyacrylic ester composite solid material;
Step (4). TiO 2 precursor/polyacrylic ester composite solid material is pulverized 5 minutes, obtained solid particulate;
Step (5). by above-mentioned solid particulate at 800 DEG C, N
2calcine 4 hours under inert atmosphere, obtain nanometer titanium dioxide titanium block material.
Embodiment 3
Step (1). 9.8g triethylene glycolbismethyl-acrylate, 0.2g gorgeous good solid 184 are uniformly mixed at 80 DEG C, obtain 10g mixed solution;
Step (2). 10g titanium isopropylate is joined in above-mentioned mixing solutions, stir 30 minutes, obtain 20g TiO 2 precursor solution;
Step (3). above-mentioned TiO 2 precursor solution is injected in mould, adopts 10W blue light illumination solidification in 100 seconds, obtain TiO 2 precursor/polyacrylic ester composite solid material;
Step (4). TiO 2 precursor/polyacrylic ester composite solid material is pulverized 2 minutes, obtained solid particulate;
Step (5). by above-mentioned solid particulate at 800 DEG C, N
2calcine 4 hours under inert atmosphere, obtain nanometer titanium dioxide titanium block material.
Embodiment 4
Step (1). 9.9g dimethacrylate glycol ether ester, 0.1g gorgeous good solid 2959 are uniformly mixed at 65 DEG C, obtain 10g mixed solution;
Step (2). 1.25g titanyl sulfate is joined in above-mentioned mixed solution, stir 15 minutes, obtain 11.25g TiO 2 precursor solution;
Step (3). above-mentioned TiO 2 precursor solution is injected in mould, adopts the solidification in 200 seconds of 20W UV Light, obtain TiO 2 precursor/polyacrylic ester composite solid material;
Step (4). TiO 2 precursor/polyacrylic ester composite solid material is pulverized 3 minutes, obtained solid particulate;
Step (5). by above-mentioned solid particulate at 700 DEG C, N
2calcine 3 hours under inert atmosphere, obtain nanometer titanium dioxide titanium block material.
Embodiment 5
Step (1). 9.85g Ethylene glycol dimethacrylate, 0.15g gorgeous good solid 907 are uniformly mixed at 70 DEG C, obtain 10g mixed solution;
Step (2). 7g titanium tetrachloride is joined in above-mentioned solution, stir 10 minutes, obtain TiO 2 precursor solution;
Step (3). above-mentioned TiO 2 precursor solution is injected in mould, adopts 20W blue light illumination solidification in 150 seconds, obtain TiO 2 precursor/polyacrylic ester composite solid material;
Step (4). TiO 2 precursor/polyacrylic ester composite solid material is pulverized 4 minutes, obtained solid particulate;
Step (5). by above-mentioned solid particulate at 700 DEG C, N
2calcine 4 hours under inert atmosphere, obtain nanometer titanium dioxide titanium block material.
Embodiment 6
Step (1). 9.98g TEG dimethacrylate and 0.02g gorgeous good solid 369 are uniformly mixed at 80 DEG C, obtain 10g mixed solution;
Step (2). 1g Butyl Phthalate and 1.9g titanium isopropylate are joined in above-mentioned solution, stirs 25 minutes, obtain TiO 2 precursor solution;
Step (3). above-mentioned TiO 2 precursor solution is injected in mould, adopts the solidification in 130 seconds of 40W UV Light, obtain TiO 2 precursor/polyacrylic ester composite solid material;
Step (4). TiO 2 precursor/polyacrylic ester composite solid material is pulverized 2 minutes, obtained solid particulate;
Step (5). by above-mentioned solid particulate at 650 DEG C, N
2calcine 3.5 hours under inert atmosphere, obtain nanometer titanium dioxide titanium block material.
Embodiment 7
Step (1). 9.8g1,6-hexanediol dimethacrylate and 0.2g gorgeous good solid 754 are uniformly mixed at 60 DEG C, obtain 10g mixed solution;
Step (2). 1.8g titanium isopropylate and 1.8g titanyl sulfate are joined in above-mentioned solution, stirs 30 minutes, obtain TiO 2 precursor solution;
Step (3). above-mentioned TiO 2 precursor solution is injected in mould, adopts 30W blue light illumination solidification in 250 seconds, obtain TiO 2 precursor/polyacrylic ester composite solid material;
Step (4). TiO 2 precursor/polyacrylic ester composite solid material is pulverized 3 minutes, obtained solid particulate;
Step (5). by above-mentioned solid particulate at 700 DEG C, N
2calcine 5 hours under inert atmosphere, obtain nanometer titanium dioxide titanium block material.
Embodiment 8
Step (1). 9.85g ethoxylated bisphenol dimethacrylate and 0.15g camphorquinone are uniformly mixed at 80 DEG C, obtain 10g mixed solution;
Step (2). 0.3g titanium isopropylate, 2g titanyl sulfate and 2g titanium tetrachloride are joined in above-mentioned solution, stirs 30 minutes, obtain TiO 2 precursor solution;
Step (3). above-mentioned TiO 2 precursor solution is injected in mould, adopts the solidification in 100 seconds of 30W UV Light, obtain TiO 2 precursor/polyacrylic ester composite solid material;
Step (4). TiO 2 precursor/polyacrylic ester composite solid material is pulverized 4 minutes, obtained solid particulate;
Step (5). by above-mentioned solid particulate at 800 DEG C, N
2calcine 3 hours under inert atmosphere, obtain nanometer titanium dioxide titanium block material.
Embodiment 9
Step (1). gorgeous to 9.8g urethanum, 0.1g good solid 1173,0.1g gorgeous good solid 184 is uniformly mixed at 80 DEG C, obtains 10g mixed solution;
Step (2). 3.7g Butyl Phthalate is joined in above-mentioned solution, stir 20 minutes, obtain TiO 2 precursor solution;
Step (3). above-mentioned TiO 2 precursor solution is injected in mould, adopts the solidification in 200 seconds of 50W UV Light, obtain TiO 2 precursor/polyacrylic ester composite solid material;
Step (4). TiO 2 precursor/polyacrylic ester composite solid material is pulverized 4 minutes, obtained solid particulate;
Step (5). by above-mentioned solid particulate at 700 DEG C, N
2calcine 3 hours under inert atmosphere, obtain nanometer titanium dioxide titanium block material.
Embodiment 10
Step (1). gorgeous to 5g dihydroxyphenyl propane-glycidyl Methacrylate, 4.8g triethylene glycolbismethyl-acrylate, 0.1g good solid 2959,0.1g gorgeous good solid 907 is uniformly mixed at 60 DEG C, obtains 10g mixed solution;
Step (2). 7.3g titanium isopropylate is joined in above-mentioned solution, stir 10 minutes, obtain TiO 2 precursor solution;
Step (3). above-mentioned TiO 2 precursor solution is injected in mould, adopts 50W blue light illumination solidification in 240 seconds, obtain TiO 2 precursor/polyacrylic ester composite solid material;
Step (4). TiO 2 precursor/polyacrylic ester composite solid material is pulverized 5 minutes, obtained solid particulate;
Step (5). by above-mentioned solid particulate at 800 DEG C, N
2calcine 2 hours under inert atmosphere, obtain nanometer titanium dioxide titanium block material.
Embodiment 11
Step (1). gorgeous for gorgeous to 2g dimethacrylate glycol ether ester, 3g Ethylene glycol dimethacrylate, 4.8g TEG dimethacrylate, 0.05g good solid 369,0.05g good solid 819,0.1g gorgeous good solid 754 is uniformly mixed at 60 DEG C, obtains 10g mixed solution;
Step (2). 3.6g titanyl sulfate is joined in above-mentioned solution, stir 30 minutes, obtain TiO 2 precursor solution;
Step (3). above-mentioned TiO 2 precursor solution is injected in mould, adopts 50W blue light illumination solidification in 60 seconds, obtain TiO 2 precursor/polyacrylic ester composite solid material;
Step (4). TiO 2 precursor/polyacrylic ester composite solid material is pulverized 5 minutes, obtained solid particulate;
Step (5). by above-mentioned solid particulate at 800 DEG C, calcine 2 hours under argon inert atmosphere, obtain nanometer titanium dioxide titanium block material.
The selection of each embodiment of table 1, comparative example Raw and the structure of final material
Above-described embodiment is not that the present invention is not limited only to above-described embodiment for restriction of the present invention, as long as meet application claims, all belongs to protection scope of the present invention.
Claims (6)
1. the preparation method of an extra small nano titanium dioxide hybrid material, it is characterized in that the method adopts thermoset bifunctional acrylate class unsaturated polyester monomer to replace conventional solvent as solvent system, titanium source is dissolved in this solvent, pass through curing unsaturated resins, obtain the blocks of solid containing TiO 2 precursor, inert atmosphere high-temperature calcination after pulverizing, because thermosetting resin is difficult to melting occurs in high-temperature burning process, so can effectively control titanium dioxide nano-particle pattern, thus obtain extra small nano titania hybrid material.
2. the preparation method of a kind of extra small nano titanium dioxide hybrid material as claimed in claim 1, is characterized in that the method comprises the following steps:
Step (1). esters of acrylic acid unsaturated polyester monomer and light trigger are uniformly mixed at 60 ~ 80 DEG C, obtain mixed solution; In mixed solution, the mass content of light trigger is 0.2 ~ 2.0 ﹪;
Step (2). titanium source is joined in above-mentioned mixed solution, stir 5 ~ 10 minutes, obtain the mixing solutions containing TiO 2 precursor; Every 10 grams contain 0.001 ~ 5 gram of titanium source containing in the mixing solutions of TiO 2 precursor;
Step (3). be injected in mould by the above-mentioned mixing solutions containing TiO 2 precursor, adopt blue light or ultraviolet light polymerization, illumination 60 ~ 240 seconds under 5 ~ 50W power, obtains TiO 2 precursor/polyacrylic ester composite solid material;
Step (5). TiO 2 precursor/polyacrylic ester composite solid material is pulverized, pulverizes 1 ~ 5 minute, obtain solid particulate;
Step (6). by above-mentioned solid particulate at 500 ~ 800 DEG C, calcine 2 ~ 6 hours under inert atmosphere, obtain extra granular nano titanium dioxide hybrid material.
3. the preparation method of a kind of extra small nano titanium dioxide hybrid material as claimed in claim 1 or 2, it is characterized in that described esters of acrylic acid unsaturated polyester monomer is one or more in dihydroxyphenyl propane-glycidyl Methacrylate, triethylene glycolbismethyl-acrylate, dimethacrylate glycol ether ester, Ethylene glycol dimethacrylate, TEG dimethacrylate, HDDMA, ethoxylated bisphenol dimethacrylate.
4. the preparation method of a kind of extra small nano titanium dioxide hybrid material as claimed in claim 2, it is characterized in that described light trigger be gorgeous good solid 1173, gorgeous good solid 184, gorgeous good solid 2959, gorgeous good solid 907, gorgeous good solid 369, gorgeous good solid 819, gorgeous good solid 754 or camphorquinone in one or several.
5. the preparation method of a kind of extra small nano titanium dioxide hybrid material as claimed in claim 1 or 2, is characterized in that described titanium source is one or several in Butyl Phthalate, titanium isopropylate, titanyl sulfate, titanium tetrachloride.
6. the preparation method of a kind of extra small nano titanium dioxide hybrid material as claimed in claim 1 or 2, is characterized in that inert atmosphere is nitrogen or argon gas.
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CN108398733A (en) * | 2018-03-08 | 2018-08-14 | 常熟理工学院 | A kind of titania/silica 1-D photon crystal and preparation method thereof |
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