WO2013029203A1 - 一种担载有二氧化钛层的无机非金属矿物复合材料、其制备方法及应用 - Google Patents
一种担载有二氧化钛层的无机非金属矿物复合材料、其制备方法及应用 Download PDFInfo
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- WO2013029203A1 WO2013029203A1 PCT/CN2011/001469 CN2011001469W WO2013029203A1 WO 2013029203 A1 WO2013029203 A1 WO 2013029203A1 CN 2011001469 W CN2011001469 W CN 2011001469W WO 2013029203 A1 WO2013029203 A1 WO 2013029203A1
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- Prior art keywords
- titanium dioxide
- composite material
- layer
- nano
- dispersant
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- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 85
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Classifications
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- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
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- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
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- C01G23/00—Compounds of titanium
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- C01G23/047—Titanium dioxide
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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Definitions
- the present invention relates to an inorganic non-metallic mineral composite material carrying a titanium dioxide layer, a preparation method and application of the composite material.
- the invention further relates to an inorganic non-metallic mineral composite material carrying a titanium dioxide layer and one or more functional layers, a method of preparation and application of the composite material. Background technique
- Titanium dioxide is an important chemical raw material closely related to our life. When its particle size drops to the nanometer level, it has a good absorption of ultraviolet light and photocatalytic properties due to its special structural level. Years of research hotspots. However, due to the large specific surface energy of nano-titanium dioxide, the application of nano-titanium dioxide in coatings, plastics, paper, rubber, environmental treatment, etc., can not achieve true nano-dispersion, and can only exist in the form of micron-sized agglomerates. In the middle, the nanometer performance cannot be fully demonstrated.
- An inorganic antibacterial composite micropowder prepared by nano-nano-titanium dioxide-coated silica is prepared, and the powder is added to an ABS resin to prepare an antibacterial polymer product; and as a patent CN101077792A, only one of the inventions by Jinfang is passed through a sol-gel method.
- the orthotitanic acid is a titanium source
- the sol-gel is obtained by dissolving ortho-titanic acid with hydrogen peroxide
- the nano-titanium composite material with a core-shell structure is prepared by coating nano-titanium dioxide on the surface of polystyrene; as in patent 101475215A, Huadong et al.
- the titanium tetrachloride or titanium sulfate is directly added dropwise to the suspension of barium sulfate or barium sulfate, and the titanium dioxide hydrate is directly hydrolyzed on the surface of barium sulfate and barium sulfate, and then dehydrated at a high temperature to obtain a composite titanium oxide.
- Wang Jing et al. invented a method for preparing a photocatalytic functional powder by supporting nano titanium dioxide on the surface of a zeolite by using zeolite as a carrier and a soluble titanium salt as a titanium source.
- the patent CN1 01 1 08335 ⁇ Guo Li et al.
- the loading rate (or coating ratio) of nano-titanium dioxide has many influencing factors, and the loading rate is low or the supporting firmness is insufficient.
- the micron-sized carrier carries nano-titanium dioxide, and the formation of a strong combination is limited by many reaction conditions.
- a method for preparing a composite material by an inorganic precipitation reaction-heat treatment crystallization process using a water-soluble titanium salt as a titanium source the process is affected by many factors such as pH, impurity ions, temperature, carrier, etc., and is often obtained by being free.
- nano titanium dioxide a mixture of nano titanium dioxide, a carrier, and a carrier carrying nano titanium dioxide; under certain conditions, a composite of nano titanium dioxide and a carrier, such as pearl mica, can be obtained, but a solid layer cannot be formed between the titanium dioxide layer and the carrier layer. Loading, the nano-titanium dioxide is easily detached from the carrier after the composite material is dispersed at a high speed.
- the inventors of the present application disclosed in CN101676030A and CN101 676031 A that the titanium tetrachloride is subjected to secondary hydrolysis under the synergistic action of hydrochloric acid and a polymer compound, and the nano titanium dioxide layer is coated on the surface of the acid-resistant non-metallic ore. No high temperature calcination is required.
- hydrochloric acid inhibits the growth of the nanoparticles during the hydrolysis of titanium tetrachloride, the size of the formed titanium dioxide nanoparticles is concentrated in the range of 10 nm, and thus the nano titanium dioxide is highly transparent, thereby limiting Titanium dioxide has a high refractive index and high hiding power performance.
- Another object of the present invention is to provide a process for preparing a composite material in which a nano-titanium dioxide layer is supported on an inorganic non-metallic mineral carrier, which is simple in process and low in preparation cost.
- It is still another object of the present invention to provide a composition comprising a composite material in which a titanium dioxide layer is supported on an inorganic non-metallic mineral support.
- Still another object of the present invention is to provide the use of a composite material in which a titanium dioxide layer is supported on an inorganic non-metallic mineral support.
- a composite material comprising inorganic non-gold as a carrier It is a mineral and a nano-titanium dioxide layer supported on the carrier.
- the layer is composed of a plurality of titanium dioxide nanospheres composed of a plurality of titanium dioxide nano-single particles.
- the present invention also provides a composite material comprising an inorganic non-metallic mineral as a carrier, a nano-titanium dioxide layer supported on the carrier, and one or more functional layers supported on the nano-titanium dioxide layer,
- the nano-titanium dioxide layer is composed of a plurality of titanium dioxide nanospheres composed of a plurality of titanium dioxide nano-single particles.
- the inorganic non-metallic mineral as a carrier is acid-resistant.
- the inorganic non-metallic mineral as a carrier is selected from the group consisting of kaolin, mica, talc, barium sulfate, diatomaceous earth, bentonite, montmorillonite, silica, wollastonite, zeolite, sepiolite, An attapulgite, one or more substances in a magnet.
- the inorganic non-metallic mineral as the carrier has a particle diameter in the range of 0.2 to 100 ⁇ ⁇ .
- the inorganic non-metallic mineral as the carrier has a particle diameter in the range of 1 - 40 ⁇ m.
- the titanium dioxide nano single particles have a diameter in the range of 1 to 20 nm, and the titanium dioxide nanospheres have a diameter of 2 to 100 times the diameter of the titanium dioxide nano single particles.
- the titanium dioxide nano single particles have a diameter in the range of 2 to 10 nm, and the titanium dioxide nanospheres have a diameter of 5 to 50 times the diameter of the titanium dioxide nano single particles.
- the nano titanium dioxide layer is supported in an amount of from 1 to 50% by weight based on the weight of the inorganic non-metallic mineral carrier layer.
- the supported amount of the nano-titanium dioxide layer is preferably from 5 to 30% by weight based on the weight of the inorganic non-metallic mineral carrier layer.
- the supported amount of the nano-titanium dioxide layer is more preferably from 5 to 20% by weight based on the weight of the inorganic non-metallic mineral carrier layer.
- the loading amount of the functional layer is 0.1 to 20% by weight of the inorganic non-metallic mineral carrier layer.
- the nano-titanium dioxide layer is firmly supported on the inorganic non-metallic mineral carrier layer.
- the firm support of the nano-titanium dioxide layer can be confirmed by the following method - 1 gram of the composite material is formulated into a 5% suspension with 20 g of ethanol, and the high-speed dispersion homogenization is performed at a rotational speed of 10,000 rpm. The machine was dispersed for 4 hours, and the concentration of the suspension was diluted to 0. 05% with ethanol, and 0. 02 ml of the diluted solution was taken as a sample, and examined by transmission electron microscopy to select regions in which the particles were distinct, uniform, and concentrated, respectively. Electron micrographs were taken at magnifications of 5,000 and 20,000. From the obtained electron micrographs, it was found that the composites were dispersed by a high-speed dispersion homogenizer, and no free titanium dioxide nanospheres were observed.
- the functional layer is selected from the group consisting of an ultraviolet shielding protective layer, a flame-retardant layer, a photocatalytic reinforcing layer, an antibacterial layer or a photocatalytic antibacterial reinforcing layer.
- the ultraviolet shielding protective layer comprises one or more oxides selected from the group consisting of silicon oxide, hydrated silicon oxide, aluminum oxide, hydrated aluminum oxide, and zirconium oxide.
- the flame retardant layer contains magnesium hydroxide.
- the photocatalytic enhancement layer comprises zinc oxide.
- the antimicrobial layer comprises a silver salt.
- the photocatalytic antimicrobial reinforcing layer comprises zinc oxide and a silver salt.
- the silver salt is selected from the group consisting of silver chloride or silver phosphate.
- a method of preparing a composite comprising an inorganic non-metallic mineral as a support and a nano-titanium dioxide layer supported on the support, the method comprising the steps of - in water, inorganic acid and A dispersion suspension of an inorganic non-metallic mineral used as a support material is prepared in the presence of a first dispersant, and a titanium tetrachloride hydrolyzate is prepared in the presence of water and a second dispersant,
- the composite suspension according to claim 1 is obtained by mixing the dispersion suspension of the acid-resistant non-metallic mineral and the titanium tetrachloride hydrolyzate to cause the reaction to be complete.
- the present invention also provides a composite material comprising an inorganic non-metallic mineral as a carrier, a nano-titanium dioxide layer supported on the carrier, and one or more functional layers supported on the nano-titanium dioxide layer.
- Method includes the following steps:
- the step (2) may be repeated to produce a composite having a multi-layer functional layer.
- the first dispersing agent is selected from the group consisting of sodium polyacrylate, ammonium polyacrylate, polyacrylamide, alkali metal polyglycolate, polycarboxylic acid, sodium polycarboxylate, and twelfth One or more of sodium sulfate, sodium dodecylsulfonate, sodium lignosulfonate, ammonium salt dispersant, polyester dispersant, polyether dispersant.
- the second dispersing agent is selected from the group consisting of polyacrylamide, polyvinyl alcohol, sodium polyacrylate, ammonium polyacrylate, polycarboxylic acid, sodium polycarboxylate, ammonium salt dispersant, polyester Minute One or more of a powder, a polyether dispersant, a polyethylene glycol type dispersant, a polyalkenyl alcohol dispersant, a polyimide type dispersant, or a polyurethane type dispersant.
- the first dispersing agent and the second dispersing agent may be the same or different.
- the inorganic non-metallic mineral suspension prepared in the presence of water, a mineral acid and a first dispersant is uniformly dispersed, and has a solid content of 4 to 50% by weight; 01 ⁇ 10 ⁇
- the suspension of the suspension is 0. 01 -10% by weight of the suspension.
- the titanium tetrachloride hydrolyzate prepared in the presence of water and a second dispersant the weight ratio of water to titanium tetrachloride is (1 - 1 0) : 1 ;
- the second dispersing agent accounts for 0.5 to 20% by weight of titanium tetrachloride.
- the mixing ratio of the inorganic non-metallic mineral suspension and the titanium tetrachloride hydrolyzate is such that titanium tetrachloride accounts for 2 to 60% by weight of the inorganic non-metallic mineral.
- the inorganic acid is an inorganic strong acid.
- the inorganic acid is one selected from the group consisting of sulfuric acid, hydrochloric acid, and nitric acid, or a mixed acid of several of them.
- a composition comprising the composite material of the invention described above.
- the composition may be a coating composition, a cosmetic composition, a papermaking composition, a binder composition, a water treatment composition, a plastic, a rubber, a fiber, a ceramic, an adhesive or a cement composition.
- the present invention also provides the industrial application of the above composite material of the present invention as an additive.
- the application is in the field of paper, plastics, paints, fibers, cosmetics, rubber, ceramics, adhesives, cement or water treatment.
- the composite material of the present invention has a special structure of the supported nano-titanium dioxide layer, the layer is composed of a plurality of titanium dioxide nanospheres, and the titanium dioxide nanospheres are further composed of a plurality of titanium dioxide nanometers. Single particles are combined.
- the titanium dioxide layer is mostly directly composed of a plurality of titanium dioxide nano single particles.
- the nano titanium dioxide layer not only can exert the advantages of high refractive index and high hiding power, but also can exert the photocatalytic activity and broaden the composite material due to the characteristics that the plurality of titanium dioxide nano single particles constitute the nanosphere.
- the application area has improved the overall performance of the final product.
- the titanium dioxide nanospheres of the present invention have greater specific surface energy than prior art titanium dioxide nanosheets of the same size, making it easier to coat other functional layers to produce functionally enhanced or multi-functional composites.
- the method for preparing the composite material has the advantages of simple process and low cost, and does not require high-temperature calcination, and can obtain a nano-titanium dioxide layer with a high loading rate, and the nano-titanium dioxide layer in the obtained composite material is firmly supported on the inorganic non-metallic mineral carrier. .
- the composite material of the present invention has a wide range of uses, for example, as an additive for use in the fields of papermaking, plastics, coatings, fibers, cosmetics, rubber, ceramics, adhesives, cement or water treatment, and has good compatibility.
- Example 1 is a transmission electron micrograph (X 10000 times) of a sericite composite material loaded with a nano-titanium dioxide layer prepared in Example 1 by transmission electron microscopy;
- Example 2 is a transmission electron micrograph (X30000 times) of a sericite composite material loaded with a nano-titanium dioxide layer prepared in Example 1 by transmission electron microscopy;
- FIG. 3 is a transmission electron micrograph (X 100000 times) of a sericite composite material loaded with a nano-titanium dioxide layer prepared in Example 1 by transmission electron microscopy;
- FIG. 5 and FIG. 6 are diagrams showing the transmission electron microscopy of the nanometer titanium dioxide layer-loaded sericite composite material prepared in Example 1 when the titanium dioxide layer is subjected to the fastness test of the titanium dioxide layer after high-speed dispersion by a high-speed homogenizer at 10,000 rpm. Photo (X 5000 times);
- Example 7 is a transmission electron micrograph (X 20000 times) of a sericite composite material loaded with a nano-titanium dioxide layer prepared in Example 1 after high-speed dispersion of a titanium dioxide layer by a high-speed homogenizer at a 10,000 rpm high speed homogenizer;
- Example 8 is a transmission electron micrograph of a kaolin composite material loaded with a nano-titanium dioxide layer prepared in Example 2 by a transmission electron microscope (X 20000 times);
- Example 10 is a transmission electron micrograph (X 50000 times) of a kaolin composite material loaded with a nano-titanium dioxide layer prepared in Example 2 by a transmission electron microscope;
- Figure 1 is a transmission electron micrograph (X 500000 times) of a kaolin composite material loaded with a nano-titanium dioxide layer prepared in Example 2 by transmission electron microscopy;
- FIG. 13 is a transmission electron micrograph (X 50000 times) of a sericite composite material loaded with a nano-titanium dioxide layer prepared in Example 3 by transmission electron microscopy;
- FIG. 15 is a transmission electron micrograph of a sericite composite material loaded with a nano-titanium dioxide layer prepared in Example 3 by a transmission electron microscope (X 200000 times)
- Figure 16 is a UV-visible diffuse reflection absorption spectrum of the functional composite obtained in Example 4. detailed description
- the nano titanium dioxide layer supported on the inorganic non-metallic mineral carrier is composed of a plurality of titanium dioxide nanospheres, which in turn are composed of a plurality of titanium dioxide nano single particles.
- the nanometer titanium dioxide layer of this structure has the characteristics of large specific surface area, high specific surface energy, and many surface dangling bonds, and fully realizes nano-scale dispersion, and truly exerts the advantages of nano titanium dioxide.
- the titanium dioxide nano-single particles have a diameter in the range of from 1 to 20 nm, and the titanium dioxide nanospheres have a diameter of from 2 to 100 times the diameter of the titanium dioxide nano-single particles. More preferably, the titanium dioxide nanosheet has a diameter in the range of 2 to 10 nm, and the titania nanosphere has a diameter of 5 to 50 times the diameter of the titania nanoparticle. Preferably, the titanium dioxide nanospheres have a diameter in the range of 50 to 150 nanometers.
- the titanium dioxide layer in the composite material of the present invention not only has ultraviolet absorption, photocatalysis, and antibacterial properties, but these nano titanium dioxide single particles have a large specific surface area and a large number of surface atoms, and these atoms are very active and easily combine with other atoms.
- By utilizing this property it is possible to easily carry the functional layer on the titanium dioxide layer to prepare a functional composite material.
- a multi-layer (including two layers) functional layer to make a multi-functional composite material.
- titanium dioxide layer There may be many functional layers supported on the titanium dioxide layer, including but not limited to: an ultraviolet shielding protective layer, a flame retardant layer, a photocatalytic reinforcing layer, an antibacterial layer or a photocatalytic antibacterial layer.
- the ultraviolet shielding protective layer comprises one or more oxides selected from the group consisting of silicon oxide, hydrated silicon oxide, aluminum oxide, hydrated aluminum oxide, and zirconium oxide.
- the nano-titanium dioxide layer functions to absorb ultraviolet rays, and the outer ultraviolet shielding layer is used to isolate and passivate the direct contact between the free radicals generated by the absorption of ultraviolet rays in the nano-titanium dioxide layer and the products in the application field, thereby preventing the free radical oxidation degradation application products. (eg resin for coatings, plastic organics, etc.). That is to say, the titanium dioxide layer and the ultraviolet shielding protective layer work together to shield ultraviolet rays.
- the flame retardant layer contains magnesium hydroxide. Further supporting magnesium hydroxide on the nano-titanium dioxide layer of the composite material of the present invention can effectively realize nano-dispersion of the magnesium hydroxide flame-retardant material, thereby obtaining a composite material having a flame-retardant function. Further, the flame-retardant layer may be further supported on the ultraviolet shielding protective layer supported on the nano-titanium dioxide layer, or the ultraviolet shielding layer may be further supported on the flame-retardant layer supported on the nano-titanium dioxide layer to form Composite material with UV shielding and flame retardant multiple functions. This composite has a wide range of uses in the plastics and coatings sector.
- the photocatalytic enhancement layer contains zinc oxide.
- the photocatalytic material (such as zinc oxide) is continuously supported on the nanometer titanium dioxide layer of the composite material of the invention, and the zinc oxide and the nano titanium dioxide layer cooperate to further The photocatalytic activity is activated to produce a photocatalytic material having superior performance.
- the antibacterial layer contains a silver salt.
- the silver salt is preferably silver chloride or silver phosphate.
- the composite material of the present invention can simultaneously carry a photocatalytic reinforcing layer and an antibacterial layer to obtain a composite material having both photocatalytic and dim light antibacterial and antifungal functions.
- a photocatalytic antibacterial layer can also be prepared by mixing a photocatalytic material and an antibacterial material, and a photocatalytic antibacterial and antifungal solution can be realized by carrying only a layer of a mixture of a photocatalytic material and an antibacterial material on the titanium dioxide layer. Anti-mildew dual function.
- the titanium dioxide nanospheres formed by combining the nano single particles have a higher refractive index, and the opacity thereof is enhanced, so that the composite material formed with the inorganic non-metallic mineral carrier itself has a higher
- the opacity can be used to replace some of the titanium dioxide in the fields of plastics, paints and the like.
- the "nano-titanium dioxide layer" according to the present invention may be a surface completely coated with an inorganic non-metallic mineral carrier, or may be a surface partially coated with an inorganic non-metallic mineral carrier.
- the surface of the carrier is substantially entirely loaded with titanium dioxide nanospheres.
- the titanium dioxide nanospheres are dispersed on the surface of the carrier, that is, a part of the carrier surface is loaded with titanium dioxide nanospheres, and a part of the carrier surface is bare.
- the degree of coating of the nano-cerium oxide layer depends on the loading of the nano-titanium dioxide layer relative to the inorganic non-metallic mineral carrier layer. The load is usually determined by different needs (including usage and cost requirements).
- the composite of the invention is prepared by dispersing an inorganic non-metallic mineral used as a support material in the presence of water, a mineral acid and a first dispersant, stirring to form a uniformly dispersed suspension. 5 ⁇ The liquid (more preferably at a temperature of 50-100 ° C), the solid content of the suspension is 4-50% by weight (more preferably 10-35 wt%), the inorganic acid accounted for 2. 5 -35 weight of the suspension 01 ⁇ 10 ⁇ % ( More preferably, it is 0.1 to 3% by weight);
- the second dispersing agent accounts for 0.5% of titanium tetrachloride.
- the second dispersing agent accounts for 0.5% of titanium tetrachloride.
- the second dispersing agent accounts for 0.5% of titanium tetrachloride. 5-10 ⁇ %;
- the second dispersing agent accounts for 0.5 to 10% by weight of titanium tetrachloride;
- the mixing ratio of the inorganic non-metallic mineral suspension and the titanium tetrachloride hydrolyzate is such that titanium tetrachloride accounts for 2 to 60% by weight of the inorganic non-metallic mineral, and particularly preferably 4 to 40% by weight.
- the composite material having the functional layer of the present invention is prepared as follows: a composite product having a nano-titanium dioxide layer supported on an inorganic non-metallic mineral carrier obtained as above is in water and first Dispersing in the presence of a dispersing agent to prepare a suspension (more preferably at 50 to 10 (with stirring at TC), the solid content of the suspension is 10-30% by weight, and the pH of the suspension is adjusted to 4 In the range of -1 1, the raw material for preparing the functional layer is added thereto, the reaction is completed, and dried by filtration to obtain a composite material in which a functional layer is further supported on the titanium dioxide layer.
- the raw materials for preparing the functional layer can be selected depending on the desired function.
- the raw material used to prepare the ultraviolet shielding protective layer may be a silicon source, an aluminum source, and/or a zirconium source.
- the silicon source may be one or a mixture of two or more of sodium silicate, water glass, and silica sol;
- the aluminum source may be one or a mixture of two or more of aluminum chloride, aluminum sulfate, sodium metaaluminate, and the like.
- the zirconium source may be one or a mixture of two or more of zirconium oxychloride, zirconium sulfate or zirconyl sulfate.
- the raw material used to prepare the flame retardant layer may be a magnesium source.
- the magnesium source may be a soluble magnesium salt such as magnesium sulfate or magnesium chloride. While the above raw materials are added to the suspension as needed, the corresponding acid, base or salt is added, and the corresponding functional layer is obtained by the reaction.
- the corresponding acid may be one or a mixture of two or more of sulfuric acid, hydrochloric acid, nitric acid;
- the corresponding base may be one or a mixture of two or more of sodium hydroxide, potassium hydroxide, ammonia;
- the corresponding salt may be chlorine Chloride salts such as potassium, sodium chloride or ammonium chloride.
- the first dispersant is selected from the group consisting of sodium polyacrylate, ammonium polyacrylate, polyacrylamide, polyalkali metal phosphate (such as sodium tripolyphosphate, sodium hexametaphosphate or sodium pyrophosphate) One or more of polycarboxylic acid, sodium polycarboxylate, sodium dodecyl sulfate, sodium dodecylsulfonate, sodium lignosulfonate, ammonium salt dispersant, polyester dispersant, polyether dispersant
- the second dispersant is selected from the group consisting of polyacrylamide, polyvinyl alcohol, sodium polyacrylate, ammonium polyacrylate, polycarboxylic acid, sodium polycarboxylate, ammonium salt dispersant, polyester dispersant (such as fatty acid polyethylene glycol ester) One or more of a dispersing agent, a polyether dispersing agent, a polyethylene glycol type dispersing agent, a polyalkeny
- the composite of the present invention can be used in the fields of papermaking, plastics, coatings, fibers, cosmetics, rubber, ceramics, adhesives, cement or water treatment.
- the method of use is substantially the same as that of the conventional pigment titanium dioxide or inorganic filler (e.g., talc, sericite, kaolin, titanium dioxide, barium sulfate, etc.), and the amount of the composite of the present invention is generally from 1 to 20% by weight.
- the composite material of the invention can be applied not only as an ordinary inorganic filler in the above-mentioned fields, but also can replace some titanium dioxide in the above-mentioned products to a certain extent, and can also impart ultraviolet shielding, flame retardancy, photocatalysis and/or antibacterial to the product. And other functions.
- 400g of 1250 mesh sericite was added to a mixed solution of 1 100 g of water, 70 g of sulfuric acid, 1.6 g of sodium hexametaphosphate, 0.4 g of polyacrylamide, and stirred at 80-9 CTC to form a uniformly dispersed Suspension; weigh 50 g of titanium tetrachloride, and add 10 g of an aqueous solution containing 3 g of polyethylene glycol 1200, 1 g of polyvinyl alcohol (PVA), 0.5 g of polyamidiamine dispersant to 4 Titanium chloride, a stable titanium tetrachloride hydrolyzate is prepared; the titanium tetrachloride hydrolyzed droplets are added to the suspension containing sericite, and after reacting for 4 hours, the filtrate is washed with water until the pH of the filtrate is close to 4, and the composite material is filtered. The cake, after drying, gives the functional composite 1.
- PVA polyvinyl alcohol
- the titanium dioxide supporting amount of the composite material obtained in Example 1 was measured by a metal aluminum reduction method to obtain a titanium dioxide supporting amount of 5%.
- the obtained composite product was dispersed in an ethanol solvent at a concentration of 0.05% to 0.1%, and ultrasonicated for 20 minutes in an ultrasonic wave to obtain a uniform suspension.
- the suspended droplets were applied to a copper mesh and observed under high power transmission electron microscopy.
- Fig. 1 to Fig. 4 are electron micrographs at magnifications of X 10000, X 30000, X 100000, and X 500000, respectively.
- the composite product obtained in Example 1 is loaded with a nano-titanium dioxide layer on the sericite carrier 1, the titanium dioxide layer being composed of a plurality of titanium dioxide nanospheres 2, which in turn are composed of a plurality of titanium dioxide nanometers.
- Single particle 3 composition Single particle 3 composition.
- the titanium dioxide nano-single particles have a diameter of 4 to 8 nm, and the titanium dioxide nanospheres have a diameter of 50 to 85 nm. In addition, no free titanium dioxide nanoparticles were found under high power transmission electron microscopy. Detecting the loading fastness of the titanium dioxide layer
- Example 1 1 g of the composite material prepared in Example 1 was formulated into a 5% suspension with 20 g of ethanol, and dispersed by a high-speed dispersing homogenizer rotating at 10,000 rpm for 4 hours, and then the concentration of the suspension was adjusted with ethanol. Diluted to 0. 05%, taking 0. 02ml of the diluent as a sample, using a transmission electron microscope to detect, select the area of the particles that are distinct, uniform and concentrated, and take the electron microscope image at the magnification of X 5000 and X 20000 respectively, and obtain the image of Figure 5 to Fig. 7 is an electron micrograph, wherein Fig. 5 and Fig. 6 show transmission electron micrographs taken at different magnifications at 5000 magnifications.
- Example 2 It can be visually seen from these photographs that the composite material obtained in Example 1 was After dispersing by the high-speed dispersing homogenizer, no obvious free titanium dioxide nanospheres appeared. This indicates that the nano-titanium dioxide layer is firmly supported on the surface of the sericite sheet.
- Example 2
- 500 grams of 800 mesh kaolin is added to 2000 grams of water, 300 grams of hydrochloric acid, 50 grams of sulfuric acid, 2 grams of sodium hexametaphosphate, 1 gram of polyether L61 (Guangzhou Chengfeida Trading Co., Ltd.) in a mixed solution, Stir at 80-90 °C to form a uniformly dispersed suspension; weigh 240 grams of titanium tetrachloride, which will contain 6 grams of polycarboxylate TH-361 (Shandong Taihe Water Treatment Co., Ltd.), 3 grams of polyethylene glycol 1200, 1 gram of polyvinyl alcohol (PVA) aqueous solution was added dropwise to 1900 g of titanium tetrachloride to prepare a stable titanium tetrachloride hydrolyzate; the titanium tetrachloride hydrolyzed droplets were added to the suspension containing kaolin, and after reacting for 6 hours, The mixture was washed with water until the pH of the filtrate reached 5 to
- the titanium dioxide supporting amount of the composite material obtained in Example 2 was measured by a metal aluminum reduction method to obtain a titanium oxide supporting amount of 19.5%.
- the obtained composite product was dispersed in an ethanol solvent at a concentration of 0.05% to 0.1%, and ultrasonicated for 20 minutes in an ultrasonic wave to obtain a uniform suspension.
- the suspended droplets were applied to a copper mesh and observed under high power transmission electron microscopy.
- Figure 8 to Figure 1 1 are the electron micrographs at magnifications of X 20000, X 30000, X 50000, X 500000 respectively.
- the composite product obtained in Example 2 was loaded with a nano-titanium dioxide layer on the kaolin carrier 4, the titania layer consisting of a plurality of titanium dioxide nanospheres 2, which in turn were composed of a plurality of titanium dioxide nano-particles.
- Single particle 3 composition The titanium dioxide nano single particles have a diameter of 2 to 10 nm, and the titanium dioxide nanospheres have a diameter of 120 to 200 nm. In addition, no free titanium dioxide nanoparticles were found under high power transmission electron microscopy.
- 600 g of 800 mesh sericite is added to 1 100 g water, 40 g hydrochloric acid, 10 g sulfuric acid, 6 g sodium hexametaphosphate, 2 g polycarboxylate GY-D06 (Suihua Chemical Science and Technology Research Institute)
- the mixed solution is stirred at 85-95 ° C to form a uniformly dispersed suspension; 200 g of titanium tetrachloride is weighed, and 1 g of polyethylene glycol 1200, 0.4 g of polyvinyl alcohol (PVA), 0.
- PVA polyvinyl alcohol
- the amount of titanium dioxide supported by the composite material obtained in Example 3 was measured by a metal aluminum reduction method to obtain a titanium dioxide supporting amount of 12%.
- the obtained composite product was dispersed in an ethanol solvent at a concentration of 0.05% to 0.1%, and ultrasonicated for 20 minutes in an ultrasonic wave to obtain a uniform suspension.
- the suspended droplets were applied to a copper mesh and observed under high power transmission electron microscopy.
- Fig. 12 to Fig. 14 are electron micrographs at magnifications of X 20000, X 50000, and X 10000, respectively. It can be seen from these photographs that the composite product obtained in Example 3 is loaded with a nano-titanium dioxide layer on the sericite carrier 1, and the titanium dioxide layer is composed of a plurality of titanium dioxide nanospheres 2, which are in turn composed of a plurality of titanium dioxide nanometers.
- Single particle 3 composition Single particle 3 composition.
- the titanium dioxide nano single particles have a diameter of 2 to 10 nm, and the titanium dioxide nanospheres have a diameter of 150 to 250 nm. In addition, no free titanium dioxide nanoparticles were found under high power transmission electron microscopy.
- Example 4 (supporting ultraviolet shielding layer)
- TC 10% sodium hydroxide to adjust the pH
- UV-visible diffuse reflection absorption of the functional composites prepared in this example was examined by UV-Vis spectroscopy (UV-Vis-NIR Spectrophotometer) according to the method of ultraviolet and visible absorption spectroscopy according to JY/T022-1996.
- the performance, the resulting spectrum is shown in Figure 15.
- the functional composite can absorb ultraviolet light having a wavelength in the range of 200-380 ntn, and thus has a good ultraviolet shielding function.
- Example 5 supporting ultraviolet shielding protective layer and flame retardant layer
- the gram of the mixture was added to the gram of water.
- Sodium polyacrylate, 0.4 g of sodium hexametaphosphate was stirred to prepare a dispersed homogenous suspension, the suspension was heated to 80 ° C, 10% sodium hydroxide was added to adjust the pH to 10, and the concentration of 120 g was 10
- a % aqueous solution of sodium silicate was added to the suspension while adding a 10% aqueous solution of sulfuric acid to maintain a pH of 10.
- the temperature is lowered to 70 ⁇
- 10% sulfuric acid solution is added to adjust the pH to 5
- 90 gram of 10% sodium metaaluminate is continuously added to the suspension
- 10% aqueous sulfuric acid solution is added to maintain the pH.
- No change after the completion of the dropwise addition, adjust the pH to 8 with 10% sodium hydroxide, maintain the pH and temperature unchanged, and add 240 g of a 15% magnesium chloride solution to the suspension, while adding 10% Sodium hydroxide, keep the pH unchanged.
- Example 6 (supporting photocatalytic enhancement layer)
- Example 7 (supporting antibacterial layer)
- Example 8 (supporting photocatalytic antibacterial layer)
- Example 9 (Application of Functional Composite 4 in Cosmetics, Application of Foundation Cream) The functional composite material 4 obtained in Example 4 was used as a cosmetic additive, and a sunscreen lotion was prepared in accordance with the following formula.
- Stearic acid, cetyl alcohol, white oil, polyoxyethylene oleate are heated to 70-75 under constant stirring. C, it is sufficiently melted or dissolved to be uniformly prepared into a uniform oil phase for use.
- the functional composite material 4 talc powder, aluminum magnesium silicate was added to 20 g of water, stirred and dispersed for 30 minutes to make it evenly dispersed, and Span-80, triethanolamine, propylene glycol, polyethylene glycol, and 37 g of water were added thereto. ⁇ , stir to 90-100 ⁇ , sterilize for 20 minutes, then cool to 70-75 ° C, prepare the desired aqueous phase system; maintain 70-75 ⁇ under stirring, slowly prepare the prepared oil phase Add the aqueous phase system to prepare an oil/water sunscreen lotion, and then slowly add the preservative and flavor.
- the prepared sunscreen lotion containing the functional composite material 4 is tested according to IS0/TR 26369: 2009 "Cosmetic - Sunscreen efficacy test method - review and evaluation of the photoprotective performance test method for sunscreen cosmetics", the sunscreen lotion The sun protection factor is SPF15. It turns out that the functional composite is added to the cosmetic and can give the product a physical sunscreen effect.
- Example 10 Application of Functional Composite Material 4 in Coatings, Exterior Wall Latex Paint as Application Example
- a latex paint was obtained in the following formulation. 129 grams of water
- Emulsion Acrona l 290 D 270 g first with talc, titanium dioxide, functional composite 4, heavy calcium carbonate, sericite, preservative, defoamer, wetting and dispersing agent, wetting agent enapon, 70 g of water Disperse at high speed on a high-speed disperser for 1 hour, then add the emulsion Acronal 290 D, filming aid, propylene glycol, thickener, 59 g of water, etc. for 1 hour, then adjust the pH to 7-8 with 25% ammonia water to prepare latex. paint. Comparative Example 1 (Latex paint using titanium dioxide as an additive)
- a latex paint was prepared in the same manner as in Example 10 except that 120 g of titanium dioxide was used instead of 80 g of titanium dioxide and 40 g of functional composite 4.
- the latex paints prepared in Example 10 and Comparative Example 1 were tested according to GB/T9755-2001 "Synthetic Resin Emulsion Exterior Wall Coatings" as follows: Performance test item Example 10 Comparative Example 1 Comparative ratio (whiteness and light color) 0.933 0.938 Drying time (dry) /h 2 hours 2 hours Water resistance (96h) No abnormality No abnormal whiteness 93.4 94.2
- Titanium dioxide 24.2 g
- Curing agent ⁇ -2833 ((Ciba- Geigy) 3 ⁇ 1 gram
- the leveling agent was pre-dispersed in an epoxy resin at a ratio of 10%, and then the mixed component was pulverized to a particle diameter of 3-5 mni.
- the epoxy resin is also pulverized to a particle diameter of 3-5 mni, and all components are pre-mixed for 10 minutes according to the formulation, and the homogeneous mixture is added to the extruder for extrusion, and the temperature in the machine chamber is 75 ° C-85. °C, the extrusion head temperature was 95 ° C, and the extrudate was cooled for fine pulverization.
- Comparative Example 2 (Powder coating using titanium dioxide as an additive)
- a powder coating was prepared in the same manner as in Example 11 except that 32.2 g of titanium dioxide was used instead of 24.2 g of titanium dioxide and 8 g of functional composite 8.
- the epoxy powder coatings prepared in Example 11 and Comparative Example 2 were respectively subjected to electrostatic spraying, and the following performance tests were performed on the coating according to the standard GB/T 21776-2008 "Guidelines for Testing Standards for Powder Coatings and Coatings", and the results were as follows: Performance Test Item Example 1 1 Comparative Example 2 Opacity (contrast ratio) 0. 941 0. 943 Whiteness 92 93 Impact resistance Positive recoil through positive and negative recoil through the appearance of smooth and smooth smooth film thickness 65-70um 65- 70um gloss ⁇ 85 ⁇ 85 sterilization rate
- Staphylococcus aureus >99% ⁇ 24% Escherichia coli >99% >31%
- Candida albicans >93% 0
- ABS resin, silicon germanium coupling agent and composite material 5 into a high-speed mixer, stir for 5 minutes, and extrude and granulate with a reaction type twin-screw extruder.
- the temperature of each section of the extruder is 200-240 ° C.
- the extruded pellets were kneaded on a two-roll mill at 150 ° C and then press-formed at a molding temperature of 170 ° C, a preheating time of 2 minutes, a dwell time of 5 minutes, and a pressure of 55 MPa.
- Comparative Example 3 plastic ABS products without composite material 5
- ABS plastic article was directly prepared in the same manner as in Example 12 without the addition of the composite material 5.
- the ABS plastic pellets prepared in Example 12 and Comparative Example 3 were compression-molded, the ABS plastic was pressed according to the standard GB/T2406-1993 "Plastics burning performance test method: Oxygen index method", "Plastics burning performance test method” : Smoke density test method” Vertical burning according to GB / T 4609-1984 test; horizontal burning press GB / T 2408-1996 test.
- Example 1 3 Application of composite material 6 chemical fiber, taking polypropylene nonwoven fabric as an example
- Titanate coupling agent 0. 1 g
- a polypropylene nonwoven fabric was directly prepared in the same manner as in Example 12 without adding the composite material 6 and the titanate coupling agent.
- antibacterial detection was carried out on Example 13 and Comparative Example 4.
- Sterilization rate Example 13 Comparative Example 4 Staphylococcus aureus>99% 0 Escherichia coli>99% 0 Candida albicans>93% 0 It can be seen that a functional composite material 6 having photocatalytic efficacy is added to the nonwoven fabric, It can impart antibacterial effect to the non-woven fabric.
- Example 14 Application of composite material 4 in paper, coated paper as an application example
- Base paper (white cardboard): Quantitative 22518 gm 2 , tightness 0.75g. m 3 , whiteness 75.72%, opacity 98.63 %, PPS roughness 7.44 ⁇ ; gloss 11.7%.
- the starch was dispersed and dispersed in 6 g of 70 ° C water.
- the two pre-dispersed raw materials prepared above and the remaining raw materials are mixed with water and stirred to prepare a 60% solid primer for use.
- kaolin 20 grams of CaC0 3 , functional composition 4 20 grams, dispersant, sodium hexametaphosphate 0.4 g, styrene-butadiene latex (SBR) dosage 13 g, hydroxymethyl cellulose (CMC) dosage 0.5 g, hard Calcium citrate 0.5 g, butanol defoamer dosage 0.2 g, octanol 0.1 g, prepared into a solid 50% topcoat, ready for use.
- SBR styrene-butadiene latex
- CMC hydroxymethyl cellulose
- the coating operation was carried out on a K303 coater with a primer coating amount of S Og/ni 2 and a top coat amount of
- Example 10 10 - 12g/m 2 . It is dried by hot air, and the drying temperature is controlled at 105 °C. The coated paper is subjected to humidity conditioning before calendering. Comparative Example 5 (The functional composite material was not added in the coated paper formulation, and the composite material of the above formula was replaced by kaolin) Primer and topcoat were prepared in the same manner as in Example 14, except that 20 g of kaolin was used instead of 20 g of composite.
- Example 14 and Comparative Example 5 The physical properties of the coated paper prepared were determined according to national standards GB - T
- the papermaking slurry is designed to be 120g/m 2 , and the weighed pulp is stirred for 1 minute, then the functional compound is added.
- Material 6, add 30% (based on dry pulp), stir for 1 minute, add 500 pptn of polyacrylamide, stir for 30 seconds, remove, and take a piece on a square-type tablet, 0.3 Mpa
- the pressure was calendered once, and the water was equilibrated at 105 ° C for 20 minutes at room temperature to obtain a functional paper having an antibacterial effect.
- Comparative Example 6 (Adding kaolin to the functional composite in the slurry 6)
- Paper was prepared by adding kaolin in the slurry in the same manner as in Example 14.
- Example 1 6 Application of functional composite material 7 in adhesive, using neoprene adhesive as an example of construction neoprene adhesive
- Antioxidant RD 2 , 2, 4-trimethyl 1, 2-dihydroquine polymer ) 2 parts
- the solid content is generally 20% - 30%, solvent 40% toluene, 30% ethyl acetate and 30% gasoline mixed solvent).
- Antioxidant RD 2, 2, 4-trimethyl 1, 2-dihydroquine polymer 2 parts
- the solid content is generally 20% - 30%, solvent 40% toluene, 30% ethyl acetate and 30% gasoline mixed solvent).
- the neoprene rubber is melted, and then the functional composite material 7, the magnesium oxide and the calcium silicate filler are mixed into the raw rubber to prepare a rubber mixture; the resin is dissolved in the solvent, and then mixed under stirring. The rubber is dissolved therein, and the other components are added together to prepare a uniform adhesive. Detection:
- Example 1 and Pair of Adhesives Proportion 7 is tested.
- the antibacterial property is tested according to GB/T21866-2008 "Antibacterial coating (paint film) antibacterial measurement method and antibacterial effect”, and the anti-mildew is tested according to JISZ 291 1-1992 "Anti-fungal test method”.
- the functional composite material can replace the inorganic filler in the adhesive as an inorganic filler in an equal amount, and the adhesive property is unchanged, and at the same time, the antibacterial and anti-mildew effect of the adhesive is imparted.
- Example 17 Application of Functional Composites 6 in Cement (Examples of cement mortars that can be applied to building facades and floor plastering mortars)
- Naphthalene type water reducing agent naphthalene sulfonate formaldehyde condensate 0. 5 kg
- Naphthalene type water reducing agent naphthalene sulfonate formaldehyde condensate 0. 5 kg
- the cement, sand, naphthalene water reducing agent and ethylene-vinyl acetate copolymer latex powder are mixed and stirred uniformly, and the prepared comparative cement slurry is coated on a 50 cm X 50 cm glass plate and naturally dried.
- the prepared cement paste-coated glass plate is cleaned for 24 hours according to GB/T 23761 -2009 "Photocatalytic Air Purifying Material Performance Test Method".
- the cement slurry to which the functional composite material 6 is added has good air purifying properties, and can be prepared as a functional product with purified air, such as coating on a building facade or a floor plastering mortar surface layer.
- Example 18 Application of Functional Composite 4 in Rubber (Taking Styrene Butadiene Rubber as an Example)
- Antioxidant AW 1g Preparation process: The raw rubber styrene-butadiene rubber 1500 is mixed in the open mill according to the thin plate of the pan, and the raw rubber, zinc oxide, tetramethylthiuram disulfide, stearic acid, N-cyclohexyl sulfide O-benzene, 4 octyloxybenzophenone, anti-aging agent AW, functional composite material 4, sulfur is uniformly thinned after being thinned several times in the mixer, and the mixing time is 12-15 minutes.
- the vulcanization point was measured by a vulcanizer, and the vulcanization condition was 153 ° C, and vulcanization was carried out at the time of the positive vulcanization point.
- a test piece of a rubber/multifunctional composite material is formed by vulcanization or molding. Comparative Example 9 (no functional composite 4, pure styrene butadiene rubber)
- the formulation was similar to that of Example 18 except that the functional composite 4 of Example 18 was removed, and pure styrene-butadiene rubber was prepared in the same manner.
- the mechanical properties of the obtained rubber test piece according to the standard GB 6037-1985 "Determination of high temperature tensile strength and elongation at break of vulcanized rubber", GB/T 528-1998 “tensile stress-strain performance”, GB/T 528-1999 “Tear Strength Test”, GB/T 7755-1987 "Vulcanized Rubber Permeability Test” The test results are as follows -
- the functional composite material 4 can significantly improve the mechanical properties of the rubber in the styrene-butadiene rubber, and at the same time, it has a certain barrier effect on the gas, and the gas permeability is reduced by 48% compared with the pure styrene-butadiene rubber.
- Example 19 Application of multifunctional composite material 8 in ceramic glaze
- Bottom glaze formula Zirconium opaque glaze for bottom glaze Component content (% by weight)
- Preparation process After spraying the glaze twice on the surface of the ceramic mud, the ceramic is placed in the furnace for sintering. During the sintering process, it is required to uniformly heat to 300 1 in one and a half hours, and keep it for one and a half hours, and continue in one and a half hours. Warm to 600 °C at a constant speed, keep warm for 1 hour and a half, then warm to 900 °C at a constant rate. After 1 hour and a half, keep warming to 1 200 °C for 2 hours, keep warm for 2 hours, turn off the heat source. It is naturally cooled to obtain an antibacterial sanitary ceramic. Comparative example 10
- Example 19 Antibacterial rate Comparative example 10 Antibacterial rate Staphylococcus aureus 96. 3% 42%
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Abstract
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PCT/CN2011/001469 WO2013029203A1 (zh) | 2011-08-31 | 2011-08-31 | 一种担载有二氧化钛层的无机非金属矿物复合材料、其制备方法及应用 |
EP11871790.9A EP2752239A4 (en) | 2011-08-31 | 2011-08-31 | COMPOSITE MATERIAL BASED ON INORGANIC NON-METALLIC MINERAL COVERED WITH TITANIUM DIOXIDE LAYER, PREPARATION METHOD AND USE THEREOF |
US13/393,533 US8728501B2 (en) | 2011-08-31 | 2011-08-31 | Composite material of inorganic nonmetallic mineral loaded with titania layer, preparation process and use thereof |
JP2014527450A JP5893740B2 (ja) | 2011-08-31 | 2011-08-31 | 二酸化チタン層を担持した無機非金属鉱物の複合材料、その製造方法および応用 |
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Also Published As
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KR101599433B1 (ko) | 2016-03-03 |
US20130052243A1 (en) | 2013-02-28 |
KR20140068129A (ko) | 2014-06-05 |
JP2014534141A (ja) | 2014-12-18 |
EP2752239A4 (en) | 2015-08-12 |
JP5893740B2 (ja) | 2016-03-23 |
US8728501B2 (en) | 2014-05-20 |
EP2752239A1 (en) | 2014-07-09 |
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