CN102442698B - Preparation method of neutral titanium dioxide sol used for anti-ultraviolet textile - Google Patents
Preparation method of neutral titanium dioxide sol used for anti-ultraviolet textile Download PDFInfo
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- CN102442698B CN102442698B CN201010505599.6A CN201010505599A CN102442698B CN 102442698 B CN102442698 B CN 102442698B CN 201010505599 A CN201010505599 A CN 201010505599A CN 102442698 B CN102442698 B CN 102442698B
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Abstract
The invention relates to a preparation method of a titanium dioxide sol, especially relates to a preparation method of the neutral titanium dioxide sol used for anti-ultraviolet textile. The method comprises the following steps: 1) adding a titanium matrix raw material in a catalyst containing organic acid, such as an aqueous solution of lactic acid; 2) performing heat treatment on the aqueous solution at the temperature of 90-100 DEG C for activating a peptization reaction to prepare an acidic titanium dioxide sol solution; 3) neutralizing the acidic titanium dioxide sol solution by alkali to obtain the titanium dioxide sol in a neutral scope. According to the invention, the preparation method provides the beneficial effects that: the preparation process is carried out in good environment, the cost is saved, the state of the prepared product is more stable and the application is wider.
Description
Technical field
The present invention relates to a kind of preparation method of TiO 2 sol, more particularly, relate to a kind of preparation method of the neutral titanium dioxide sol for Ultraviolet Resistant Textiles.
Background technology
Ultraviolet radiation UVR comprises three types: UV-A (315-400nm), UV-B (290-315nm), and UV-C (100-290nm).UV-C radiation is absorbed by ozonosphere, UV-A and UV-B then arrives earth surface.Along with the Greenhouse effect be on the rise and depletion of the ozone layer phenomenon, the ultraviolet total amount arriving earth surface increases.A small amount of ultraviolet radiation is useful to the mankind, but a large amount of ultraviolet radiations may cause serious health problem, such as sunburn, the too early ageing of skin, even skin carcinoma and cataract.Therefore, skin needs to prevent from suffering excessive ultraviolet radiation, and especially uv b radiation, because it has the highest skin injury ability.Recently, due to ultraviolet radiation preventing and the market requirement of lightweight comfort clothes is growing, Ultraviolet Resistant Textiles receives special concern.
Clothes is considered to the VIO (Very Important Object) preventing from tanning severely and prevent skin carcinoma.But weave, the weight of clothes are different with color, effect of its ultraviolet radiation preventing is also different, and particularly some, textiles did not have enough ultraviolet radiation preventing effects in summer.Design and improve fabric to reduce that ultraviolet penetrates be a relatively new application.Usual people utilize SPF (sun protection factor) SPF to measure the ultraviolet radiation preventing ability of sun care preparations.On the other hand, the antiultraviolet coefficient UPF defined by Australia/New Zealand Standard AS/NZL 4399:1966, is nowadays also widely adopted.UPF is mainly for assessment of the ultraviolet radiation preventing ability of textiles.UPF is divided into Three Estate: UPF value is that the fabric of 15 to 24 (grade is 15 and 20) provides good ultraviolet radiation preventing ability; UPF value is that the fabric of 25 to 39 (grade is 25,30 and 35) provides good ultraviolet radiation preventing ability; UPF value be 40 and the fabric of higher (grade be 40,45,50 and 50+) fabulous ultraviolet radiation preventing ability is provided.UPF value lower than 15 fabric not within scope of assessment.
At works such as J.H.Xin, " textile research (Textile Research Journal) ", 72,97 (2004); The work such as P.Xu, " applied polymer science (Journal of Applied Polymer Science) ", 102,1478 (2006); The work such as N.Abidi, " applied polymer science (Journal of AppliedPolymer Science) ", 104, once reported in 111 (2007) and utilized titania nanoparticles process cotton fabric.But this preparation method is using tetra isopropyl titanium, tetrabutyl titanium and tetraethyl-titanium as raw material, using hydrochloric acid and acetic acid as catalyzer, in spirit solvent, carry out sol gel reaction.The preparation process of the method is not environmental friendliness, and owing to using a large amount of strong acid can pollute environment.
U.S. Patent number be 6576589 (Na etc.) patent discloses a kind of method preparing the anatase titanium dioxide of Nano Particle, using nitric acid as catalyzer, temperature controls, at 80 ± 20 DEG C, in spirit solvent, to carry out sol gel reaction.The method, due to containing caustic acid, be not environmental friendliness, and the pH value of products therefrom is less than 3, cannot be used for low acidproof material.
U.S. Patent number be 7255847 (Daoud etc.) patent describes a kind of method preparing the anatase titanium dioxide of Nano Particle, using nitric acid and hydrochloric acid as catalyzer, temperature controls, at 50 ± 15 DEG C, in water solvent, to carry out sol gel reaction.The pH value of the method products therefrom is 1-2, can cause damage to low acidproof material.
U.S. Patent number be 5049309 (Sakamoto etc.) patent discloses a kind of process for the production of neutral titanium dioxide sol.This process comprises: with monoprotic acid than example hydrochloric acid, nitric acid, chloric acid, Mono Chloro Acetic Acid peptization hydrous titanium, obtain acidic titania colloidal sol, then utilizes ion exchange resin to remove the negatively charged ion in this acidic titania colloidal sol.But the dispersiveness of the method on TiO 2 sol affects to some extent and TiO 2 sol cannot be made to be in stable dispersion state.
In sum, prior art prepares TiO 2 sol many weak points: in preparation process, adopts corrosive chemical, such as nitric acid and hydrochloric acid; Need relatively high temperature.The product prepared, carbonic acid gas nano particle or TiO 2 sol are in unstable dispersion state; And the acidic titania colloidal sol containing corrosive chemical, can not be used for some low acidproof materials, such as fiber textile.
Summary of the invention
The technical problem to be solved in the present invention is; for prior art employing corrosive chemical, need relatively high temperature, the carbonic acid gas nano particle of acquisition or TiO 2 sol is unstable and the application of acidic titania colloidal sol is wideless defect, a kind of preparation method of the neutral titanium dioxide sol for Ultraviolet Resistant Textiles is provided.
The technical solution adopted for the present invention to solve the technical problems is: the preparation method constructing a kind of neutral titanium dioxide sol for Ultraviolet Resistant Textiles, comprises the following steps:
1) titanium based raw material is added to comprise in the aqueous solution of organic acid catalyst;
2) the described aqueous solution is heat-treated activate peptization reaction, thus prepare acidic titania sol solution;
3) use in alkali and described acidic titania sol solution, thus obtain the TiO 2 sol in neutral range.
In the preparation method of the neutral titanium dioxide sol for Ultraviolet Resistant Textiles of the present invention, described step 1) in described organic acid catalyst be lactic acid.
In the preparation method of the neutral titanium dioxide sol for Ultraviolet Resistant Textiles of the present invention, described step 1) in described titanium based raw material be selected from one or more mixtures in race, and described race comprises: purity titanium tetraethoxide, tetraisopropoxy titanium, four titanium butoxide, titanium chloride, titanium sulfate and slag titanium sulfate.
In the preparation method of the neutral titanium dioxide sol for Ultraviolet Resistant Textiles of the present invention, described step 2) described in prepare acidic titania sol solution peptization reaction carry out in the temperature of 90-100 DEG C.
In the preparation method of the neutral titanium dioxide sol for Ultraviolet Resistant Textiles of the present invention, described step 3) in described alkali be selected from mineral alkali and organic bases.
The neutral titanium dioxide sol for Ultraviolet Resistant Textiles prepared by preparation method of the present invention, comprises the titanium oxide colloid particle that weight percent is 1-20%.
Implement the preparation method of the neutral titanium dioxide sol for Ultraviolet Resistant Textiles provided by the invention, there is following beneficial effect: the process of preparation is carried out in aqueous, do not use aggressive solvent, and without the need to high-temperature heat treatment, also without the need to high pressure, therefore process environment close friend, saving cost; The product of preparation is neutral titanium dioxide sol, is in stable dispersion state, and can be used on low acidproof material, such as textiles, plastics, timber, paper, and therefore Product Status is more stable, application is more extensive.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing:
Fig. 1 is the performance diagram of untreated white plain weave cotton fabric and the white plain weave cotton fabric antiultraviolet through 0.5% titanium dioxide process of the preferred embodiment of the present invention;
Fig. 2 is the performance diagram of untreated white twill cotton fabric and the white twill cotton fabric antiultraviolet through 0.5% titanium dioxide process of the preferred embodiment of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in more detail.
The method that the present invention prepares neutral titanium dioxide antiultraviolet film comprises the following steps: added to by titanium based raw material and comprise in the aqueous solution of organic acid catalyst; The aqueous solution is carried out to the thermal treatment of 90-100 DEG C to activate peptization reaction, thus prepare acidic titania sol solution; With in alkali and acidic titania sol solution, thus obtain the TiO 2 sol in neutral range; By neutral titanium dioxide sol coating on material.
TiO 2 sol prepared by the present invention is the water dispersion within the scope of a neutral pH, and titanium dioxide granule is dispersed in this water dispersion.The pH value of described TiO 2 sol can regulate as required.Can be titanium alcoholate, titanium chloride, titanium sulfate for making the titanium based raw material of collosol intermixture, such as tetra isopropyl titanium, four titanium butoxide, titanium tetrachloride, titanyl sulfate.In this case, the direct hydrolysis of alkoxide can produce oxyhydroxide.Then there is polycondensation, produce titanium oxide.Utilize organic acid, such as lactic acid is as the catalyzer of titanium based raw material hydrolysis reaction and condensation reaction.
Preparation in accordance with the present invention, by a certain amount of titanium based raw material, slowly add in suitable quantity of water, the appropriate organic acid catalyst for improving reactivity is comprised in this water, subsequently this mixture is stirred at the temperature of 90-100 DEG C, and continue the appropriate peptization reaction times, such as about 2 to 4 hours.The time length of this peptization reaction is optional, depends on phase and the size of crystal completely.In preparation method, the time length of peptization reaction can increase along with the increase of titanium based raw material.This is because need the time relatively grown allow the crystallization of a large amount of titanium based raw material.Can be mineral alkali or organic bases for neutralizing the alkali of acid titania solution, such as sodium hydroxide, ammonia, thanomin.
Adopt different deposition techniques, by neutral titanium dioxide sol liquid coating on material, such as, dip-coating, spin coating, spraying etc.Then, this material require for some time is dry or bake in lesser temps in atmosphere, forms inorganic network structure and makes coating become fine and close, thus improve the adhesive power of neutral titanium dioxide sol at material surface.The time that bakes after coating and baking temperature are completely optional.
In a preferred embodiment of the invention, following three aspects are comprised.
One, the preparation of neutral titanium dioxide sol
600ml deionized water is housed in 2000ml beaker, wherein comprises 25ml lactic acid, churned mechanically while, 375ml tetra isopropyl titanium is added in this deionized water lentamente.While continuation is stirred, this mixture is heated to 90 degrees Celsius and continues 4 hours.Then this mixture is remained on 90 DEG C, and add thanomin wherein to regulate the pH value of this mixture to 6-7.Last while stir this mixing solutions, allow it be cooled to room temperature.Result obtains water white mixing solutions.
Two, process is arranged
The mixing solutions that the above results obtains is TiO 2 sol, is used for making titanium deoxid film, by the process of soaking-rolling-drying-baking, covers white plain weave and twill surface of cotton fabric respectively.The white plain weave of 10 × 10cm and twill cotton fabric are immersed in this TiO 2 sol respectively, then utilize automatic padding machine to pad respectively.The fabric padded is dried 2 minutes in the pre-heating drying machine of 80 DEG C, finally in the preheating baker of 120 DEG C, bakes 3 minutes.
Three, antiultraviolet characteristic
Antiultraviolet coefficient UPF directly can assess the ultraviolet radiation preventing ability of textiles.Fig. 1 and Fig. 2 respectively illustrates the rational curve of the white plain weave of 0.5% titanium dioxide process through above-mentioned making and the antiultraviolet of twill cotton fabric, and is compared by the rational curve of itself and untreated white plain weave and twill cotton fabric antiultraviolet respectively.
Referring to Fig. 1, is the performance diagram of untreated white plain weave cotton fabric and the white plain weave cotton fabric antiultraviolet through 0.5% titanium dioxide process of the preferred embodiment of the present invention.As shown in Figure 1, the rational curve of untreated white plain weave cotton fabric antiultraviolet is (a), and the rational curve through the white plain weave cotton fabric antiultraviolet of 0.5% titanium dioxide process of the preferred embodiment of the present invention is (b).From UPF value, untreated cotton fabric UPF value is 5, and treated cotton fabric UPF value is 18.Penetrate peak value from ultraviolet, it is 25% that untreated cotton fabric ultraviolet penetrates peak value, and it is 22% that treated cotton fabric ultraviolet penetrates peak value.Integrated comparative, treated cotton fabric is higher than untreated cotton fabric UPF value, and ultraviolet to penetrate peak value lower.
Referring to Fig. 2, is the performance diagram of untreated white twill cotton fabric and the white twill cotton fabric antiultraviolet through 0.5% titanium dioxide process of the preferred embodiment of the present invention.As shown in Figure 2, the rational curve of untreated white twill cotton fabric antiultraviolet is (a), and the rational curve through the white twill cotton fabric antiultraviolet of 0.5% titanium dioxide process of the preferred embodiment of the present invention is (b).From UPF value, untreated cotton fabric UPF value is 8, and treated cotton fabric UPF value is 52 and UPF grade is 50.Penetrate peak value from ultraviolet, it is 18% that untreated cotton fabric ultraviolet penetrates peak value, and it is 16% that treated cotton fabric ultraviolet penetrates peak value.Integrated comparative, treated cotton fabric is higher than untreated cotton fabric UPF value, and ultraviolet to penetrate peak value lower.
Incorporated by reference to consulting Fig. 1 and Fig. 2, can find out that fabric is after the 0.5% titanium dioxide process that the preparation method of the preferred embodiment of the present invention obtains, UPF value increases and ultraviolet penetrates peak value reduces, and illustrates that the characteristic of fabric antiultraviolet is improved.This is because Nano titanium dioxide particle can absorb and uv reflectance consumingly.
Implement the preparation method of the neutral titanium dioxide sol for Ultraviolet Resistant Textiles provided by the invention, there is following beneficial effect:
The process of preparation is carried out in aqueous, does not use aggressive solvent, and without the need to high-temperature heat treatment, also without the need to high pressure, therefore process environment close friend, saving cost; The product of preparation is neutral titanium dioxide sol, is in stable dispersion state, and can be used on low acidproof material, such as textiles, plastics, timber, paper, and therefore Product Status is more stable, application is more extensive.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every equivalent structure transformation utilizing specification sheets of the present invention and accompanying drawing content to do, or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (1)
1. for a preparation method for the neutral titanium dioxide sol of Ultraviolet Resistant Textiles, it is characterized in that, comprise the following steps:
1) the one or more mixtures in purity titanium tetraethoxide, tetraisopropoxy titanium, four titanium butoxide, titanium chloride, titanium sulfate and slag titanium sulfate are added in the aqueous solution comprising lactic acid catalyzer;
2) heat-treat the described aqueous solution and activate peptization reaction, peptization reaction is carried out in the temperature of 90-100 DEG C, thus prepares acidic titania sol solution;
3) with in mineral alkali or organic bases and described acidic titania sol solution, thus obtain in neutral range, comprise the TiO 2 sol that weight percent is 1-20%.
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