CN106315670A - Dispersible wedge nano titanium dioxide, and preparation method and application thereof - Google Patents
Dispersible wedge nano titanium dioxide, and preparation method and application thereof Download PDFInfo
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- CN106315670A CN106315670A CN201510758720.9A CN201510758720A CN106315670A CN 106315670 A CN106315670 A CN 106315670A CN 201510758720 A CN201510758720 A CN 201510758720A CN 106315670 A CN106315670 A CN 106315670A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention relates to a dispersible wedge nano titanium dioxide, and a preparation method and application thereof, belonging to the technical field of nano materials. The preparation method comprises the following steps: (1) in an ice water bath, adding TiCl4 into a hydrochloric acid solution while stirring; (2) dissolving COOH/CONH2-containing organic matters in ethanol or adding silane and ammonia water into the solution in the step (1), and reacting at 60-80 DEG C for 8-24 hours; and (3) after the reaction finishes, carrying out after-treatment. The dispersible wedge nano titanium dioxide particles prepared by the method can be repeatedly dispersed in water, ethanol, DMF (N,N-dimethylformamide), chloroform, acetone and various other solvents. The dispersible wedge nano titanium dioxide has favorable dispersibility in a polyurethane leather finishing agent, and can obviously enhance the water resistance, anti-friction property and weather resistance of the polyurethane leather finishing agent. The dispersible wedge nano titanium dioxide can be used as a functional additive and modifier of the polyurethane leather finishing agent. The preparation method has the advantages of simple technique, controllable reaction process and cheap and accessible raw materials, and has favorable industrial application prospects.
Description
Technical field
The invention belongs to field of nanometer material technology, be specifically related to a kind of dispersible wedge shape nano titanium oxide, its preparation method and application.
Background technology
Nano-TiO2Deeply favored by chemist with its superior photoelectric properties, Heat stability is good, persistence length, low price and the feature such as harmless, but nano-TiO2
Particle diameter be only the 1/10 of ordinary titanium powder, owing to its particle diameter is little, specific surface area big, surface energy is high and easily reunites, it is impossible to is dispersed stably in and causes separated in dielectric solvent and polymeric matrix, make its due performance be difficult to play, greatly limit nano-TiO2Application in every field.It is always, about the agglomeration traits of nano-powder, the problem that scientific worker pays close attention to most, is also basic research problem indispensable in current R and D new material.Use molecular weight height, the coating material of ad hoc structure, in the way of chemical bonding, nanoparticle is carried out surface modification, easily form certain physical barrier on the surface of nanoparticle, prevent it from assembling, good stability and cladding ability are strong, can significantly improve or change dispersibility and the compatibility of powder body, improve surface activity, make nano-particle surface produce new physics, chemistry and optical characteristics, adapt to different application requirements.
Summary of the invention
It is an object of the invention to provide a kind of dispersible wedge shape nano titanium oxide, its preparation method and application.
Based on above-mentioned purpose, the present invention adopts the following technical scheme that:
The preparation method of a kind of dispersible wedge shape nano titanium oxide, comprises the steps:
(1) in ice-water bath, by TiCl under stirring4Adding in hydrochloric acid solution, stirring to solution is water white transparency shape；
(2) will be containing COOH or CONH2Organic substance be dissolved in ethanol, join in the solution in step (1)；Or silane and ammonia are joined in the solution in step (1), react 8 ~ 24h at 60 ~ 80 DEG C；
(3) after reaction terminates, wash respectively 2 ~ 5 times with ethanol and deionized water successively, be dried, to obtain final product.
Preferably, in step (1), the concentration of hydrochloric acid solution is 1 ~ 6mol/L.
Containing COOH or CONH2Organic substance or the consumption of silane be TiCl4The 10 ~ 30% of quality, the consumption of ammonia is TiCl4The 40 ~ 70 of quality
%。
The dispersible wedge shape nano titanium oxide that above-mentioned preparation method prepares.
It should be noted that containing COOH or CONH2Organic substance or silane can also add after fully washing removes by-product, then react 8 ~ 24h at 60 ~ 80 DEG C.
Test confirms, this surface with wedge structure modifies and modified nano-titanium dioxide microgranule can be scattered in the various solvents such as water, ethanol, DMF (DMF), chloroform and acetone repeatedly.Good dispersion in polyurethane, can significantly improve water-fast, antifriction and the weatherability of polyurethane decorative paint for leather；Can be as the functional additive of polyurethane decorative paint for leather and modifying agent.Present invention process is simple, and the easily operated control of course of reaction, raw materials is cheap and easy to get, has preferable prospects for commercial application.
Accompanying drawing explanation
Fig. 1 dispersibles the FTIR spectrum figure (embodiment 3) of wedge shape nano titanium oxide；
Fig. 2 dispersibles the X-ray diffraction spectrogram (embodiment 3) of wedge shape nano titanium oxide；
Fig. 3 is the dispersibility photo in different solvents medium of the wedge shape nano titanium oxide obtained by embodiment 3, and wherein, wedge shape nano titanium oxide mass percent in different solvents is 3 %-5 %, stands and produces without precipitation for more than one month；
Fig. 4 be the wedge shape nano titanium oxide that embodiment 3 prepares transmission electron microscope under photo；
The atomic force microscope pattern collection of illustrative plates of dispersible wedge shape nano titanium oxide/Aqueous Polyurethane Leather Finishing Agent complex (b) that Fig. 5 Aqueous Polyurethane Leather Finishing Agent (a) prepares with embodiment 3 (compare pure polyurethane decorative paint for leather surface roughness and significantly increase by composite surface roughness, illustrating that dispersible wedge shape nano titanium oxide changes surface texture and the pattern of finishing agent, the raising of composite surface antifriction performance is owing to nano titanium dioxide particles is caused by the rolling effect on surface)；
Fig. 6 polyurethane decorative paint for leather resistance to water is with dispersibling wedge shape nano-TiO2The variation diagram (weight-loss ratio is the lowest, and resistance to water is the best, accounts for the percentages of polyurethane finishing agent quality with wedge shape nano titanium oxide, and its content is respectively 0 %, 1.0 %, 2.0 %, 3.0 %, 4.0 %, 6.0 %) of (embodiment 3) addition；
Fig. 7 polyurethane decorative paint for leather uv absorption is with dispersibling wedge shape nano-TiO2(interpolation dispersibles wedge shape nano-TiO in the change of (embodiment 3) addition2The uv absorption of rear finishing agent strengthens, and accounts for the percentages of polyurethane finishing agent quality with wedge shape nano titanium oxide, and its content is respectively 0 %, 0.5 %, 1.0 %, 2.0 %, 3.0 %, 4.0 %, 5.0%, 6.0 %)；
The pure polyurethane decorative paint for leather of Fig. 8 (WPU) and interpolation dispersible wedge shape nano-TiO2Polyurethane decorative paint for leather (the TiO of (embodiment 3)2/ WPU, accounts for the percentages of polyurethane finishing agent quality with wedge shape nano titanium oxide, and its content is 3 %) coefficient of friction comparison diagram.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme is described in further detail, but protection scope of the present invention is not limited thereto.
Embodiment 1
The preparation method of a kind of dispersible wedge shape nano titanium oxide, comprises the steps:
(1) in ice-water bath, by 1 mL under stirring
TiCl4Being slowly added in 50 mL hydrochloric acid solutions (1 mol/L), stirring is to water white transparency shape；
(2) 0.50 is weighed
The oxybenzoic acid (No. CAS: 69-72-7) of g, is dissolved in 20 mL dehydrated alcohol, joins in the solution of step (1), obtain orange-yellow translucent solution, be warming up to 60 DEG C, insulation reaction 8 hours；
(3) after reaction terminates, centrifugation 5 minutes (7000 revs/min), lower floor's solid is washed each 3 times respectively with dehydrated alcohol and deionized water successively, 60 DEG C are dried 12 h, obtain yellow product.
Embodiment 2
The preparation method of a kind of dispersible wedge shape nano titanium oxide, comprises the steps:
(1) in ice-water bath, by 1 mL under stirring
TiCl4Being slowly added in 50 mL hydrochloric acid solutions (2mol/L), stirring is to water white transparency shape；
(2) 0.48 is weighed
The 4-octyl benzoic acid (No. CAS: 3575-31-3) of g, is dissolved in 20 mL dehydrated alcohol, joins in the solution of step (1), obtain the translucent solution of yellow, be warming up to 70 DEG C, insulation reaction 12 hours；
(3) after reaction terminates, centrifugation 5 minutes (7000 revs/min), lower floor's solid is washed each 3 times respectively with dehydrated alcohol and deionized water successively, 60 DEG C are dried 12 h, obtain yellow product.
Embodiment 3
The preparation method of a kind of dispersible wedge shape nano titanium oxide, comprises the steps:
(1) in ice-water bath, by 1mL under stirring
TiCl4 Being slowly added in 50 mL hydrochloric acid solutions (3mol/L), stirring is to water white transparency shape；
(2) 0.36 is weighed
The 4-n-dodecane yl benzoic acid (No. CAS: 21021-55-6) of g, is dissolved in 20 mL dehydrated alcohol, joins in the solution of step (1), obtain the translucent solution of yellowish-brown；It is warming up to 80 DEG C, insulation reaction 24 hours；
(3) reaction terminates, centrifugation 5 minutes (7000 revs/min), lower floor's solid is respectively washed 3 times with dehydrated alcohol and deionized water respectively, 70 DEG C are dried 12 h, obtain light yellow product, confirm that gained light yellow product is nano titanium oxide through FTIR spectrum figure (Fig. 1) and X-ray diffraction spectrogram (Fig. 2), Fig. 4 is shown in by the electron micrograph of product, as shown in Figure 4, gained nano titanium oxide be shaped as wedge shape, product dispersibility photo in several solvents is as shown in Figure 3, wherein, wedge shape nano titanium oxide mass percent in different solvents is 3 %-5 %, stand and produce without precipitation for more than one month.
Embodiment 4
The preparation method of a kind of dispersible wedge shape nano titanium oxide, comprises the steps:
(1) in ice-water bath, by 1 mL under stirring
TiCl4Being slowly added in 50 mL hydrochloric acid solutions (5mol/L), stirring is to water white transparency shape；
(2) 0.51 is weighed
G methacryloxypropyl three (trimethylsiloxane group) silane (No. CAS: 17096-07-0) and 0.9 mL ammonia (ammonia concn is 25-28wt %), join in the solution of step (1), be warming up to 70 DEG C, insulation reaction 10 hours；
(3) after reaction terminates, centrifugation 5 minutes (7000 revs/min), lower floor's solid is respectively washed 3 times with dehydrated alcohol and deionized water respectively, 80 DEG C are dried 8 h, obtain white products.
Embodiment 5
The preparation method of a kind of dispersible wedge shape nano titanium oxide, comprises the steps:
(1) in ice-water bath, by 1 mL under stirring
TiCl4Being slowly added in 50 mL hydrochloric acid solutions (4mol/L), stirring is to water white transparency shape；
(2) 0.35 is weighed
G polyacrylamide (No. CAS:
9003-05-8, molecular weight 2,000,000), it is dissolved in 20 mL dehydrated alcohol, joins in the solution of step (1), be warming up to 80 DEG C, insulation reaction 14 hours；
(3) after reaction terminates, centrifugation 5 minutes (7000 revs/min), lower floor's solid is respectively washed 3 times with dehydrated alcohol and deionized water respectively, 70 DEG C are dried 10 h, obtain white products.
Embodiment 6
The preparation method of a kind of dispersible wedge shape nano titanium oxide, comprises the steps:
(1) in ice-water bath, by 1 mL under stirring
TiCl4Being slowly added in 50 mL hydrochloric acid solutions (6mol/L), stirring is to water white transparency shape；Being warming up to 80 DEG C, insulation reaction 8 hours, reaction terminates, and respectively washs 3 times with dehydrated alcohol and deionized water respectively；
(2) gained filter cake is redispersed in (V in the mixed liquor of 80 mL dehydrated alcohol and deionized waterDehydrated alcohol/VDeionized water=50/1) 1.3, it are subsequently adding
ML ammonia (ammonia concn is 25-28wt %), and 0.20
G octadecyl trimethoxysilane (No. CAS: 3069-42-9), stirring reaction 12 h at 50 DEG C,
(3) after reaction terminates, centrifugation 5 minutes (7000 revs/min), lower floor's solid product is washed 3 times respectively through dehydrated alcohol and deionized water, 80 DEG C are dried 9 h, obtain white products.
Application test
(Foshan Shi Telang Chemical Co., Ltd. produces to add the dispersible wedge shape nano titanium oxide that embodiment 3 prepares to 30 g Aqueous Polyurethane Leather Finishing Agents, working substance content is 30wt %) in, first strong stirring 1 h under room temperature, mix homogeneously, again by mixed liquor supersound process 10 min, sol evenning machine is used to be spin-coated on clean microscope slide by gained complex liquid, natural drying film forming.Preparing wedge shape nano titanium oxide percentage composition respectively is 0 %, 0.5 %, 1.0 %, 2.0 %, 3.0 %, 4.0 %, 5.0 %, 6.0 %(are with the percentages of shared polyurethane finishing agent quality) compelx coating sample, standby, and test its water-fast (see figure 6), antifriction and weather resistance, it will be appreciated from fig. 6 that the weight-loss ratio of polyurethane decorative paint for leather is with dispersibling wedge shape nano-TiO2The increase of addition and step-down, weight-loss ratio is the lowest, and resistance to water is the best, and wherein, when addition is 3%, the resistance to water of polyurethane decorative paint for leather is best.As shown in Figure 7, interpolation dispersibles wedge shape nano-TiO2(account for the percentages of polyurethane finishing agent quality with wedge shape nano titanium oxide, its content is respectively 0 %, 0.5 %, 1.0 % in the uv absorption enhancing of rear finishing agent, 2.0 %, 3.0 %, 4.0 %, 5.0%, 6.0 %), absorptivity increases, and transmitance declines, and nano-TiO is described2Ultraviolet light being had shielding, can improve the anti-ultraviolet property of finishing agent, i.e. weatherability, wherein, when addition is 4 .0 %, the ultraviolet absorption ability of polyurethane decorative paint for leather is the strongest.Pure polyurethane decorative paint for leather (WPU) and interpolation dispersible wedge shape nano-TiO2Polyurethane decorative paint for leather (the TiO of (embodiment 3)2/ WPU, accounts for the percentages of polyurethane finishing agent quality with wedge shape nano titanium oxide, and its content is 3 %) coefficient of friction comparison diagram see Fig. 8, as shown in Figure 8, add dispersible wedge shape nano-TiO2The coefficient of friction of polyurethane decorative paint for leather less, i.e. add and dispersible wedge shape nano-TiO2The antifriction performance of polyurethane decorative paint for leather more preferable.
Claims (5)
1. the preparation method of a dispersible wedge shape nano titanium oxide, it is characterised in that comprise the steps:
(1) in ice-water bath, by TiCl under stirring4Adding in hydrochloric acid solution, stirring to solution is water white transparency shape；
(2) will be containing COOH or CONH2The Organic substance of substituent group is dissolved in ethanol, joins in the solution in step (1)；Or silane and ammonia are joined in the solution in step (1), react 8 ~ 24h at 60 ~ 80 DEG C；
(3), after reaction terminates, solid-liquid separation product, gained solid washs 2 ~ 5 times respectively with ethanol and deionized water successively, is dried, to obtain final product.
The preparation method of dispersible wedge shape nano titanium oxide the most according to claim 1, it is characterised in that in step (1), the concentration of hydrochloric acid solution is 1 ~ 6mol/L.
The preparation method of dispersible wedge shape nano titanium oxide the most according to claim 1, it is characterised in that containing COOH or CONH2The Organic substance of substituent group or the consumption of silane are TiCl4The 10 ~ 30% of quality, the consumption of ammonia is TiCl440 ~ 70 % of quality.
4. use the arbitrary described method of claims 1 to 3 to prepare the dispersible wedge shape nano titanium oxide of gained.
5. the application in leather finishing agent of the dispersible wedge shape nano titanium oxide described in claim 4.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116640505A (en) * | 2023-06-12 | 2023-08-25 | 中轻检验认证有限公司 | Functional photo-curable leather finishing agent system and preparation method and application thereof |
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2015
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| CN1733610A (en) * | 2005-04-18 | 2006-02-15 | 江苏大学 | Method for preparing rutile type nanometer Ti02 in low temperature using carboxylic acid as finishing agent |
| US20120276389A1 (en) * | 2009-09-10 | 2012-11-01 | The National Titanium Dioxide Co., Ltd. (Cristal) | Titanium dioxide nanoparticles |
| CN103130268A (en) * | 2013-03-21 | 2013-06-05 | 南京工业大学 | High-efficiency nanocrystal titanium dioxide preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116640505A (en) * | 2023-06-12 | 2023-08-25 | 中轻检验认证有限公司 | Functional photo-curable leather finishing agent system and preparation method and application thereof |
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