CN112603838B - Nano titanium dioxide slurry oil and preparation method and application thereof - Google Patents
Nano titanium dioxide slurry oil and preparation method and application thereof Download PDFInfo
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/29—Titanium; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0241—Containing particulates characterized by their shape and/or structure
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/25—Silicon; Compounds thereof
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/58—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing atoms other than carbon, hydrogen, halogen, oxygen, nitrogen, sulfur or phosphorus
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/89—Polysiloxanes
- A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
- A61K8/894—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone modified by a polyoxyalkylene group, e.g. cetyl dimethicone copolyol
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
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- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
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- A61K2800/413—Nanosized, i.e. having sizes below 100 nm
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- A61K2800/60—Particulates further characterized by their structure or composition
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- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/60—Particulates further characterized by their structure or composition
- A61K2800/61—Surface treated
- A61K2800/62—Coated
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Abstract
The invention relates to the field of cosmetics, in particular to nano titanium dioxide slurry oil and a preparation method and application thereof. According to the invention, the silicon dioxide protective film on the surface of the nano titanium dioxide can improve the weather resistance of the nano titanium dioxide, and meanwhile, the reactive sites on the surface of the powder are increased, so that the surface of the powder is easier to be modified by other modified groups; surface-modified
Description
Technical Field
The invention relates to the field of cosmetics, in particular to nano titanium dioxide slurry oil and a preparation method and application thereof.
Background
The nano titanium dioxide has the effect of absorbing and reflecting ultraviolet rays, and is one of widely used physical sunscreens. However, because the specific surface area of the nano titanium dioxide is large, agglomeration is easy to occur, and the use is affected, the nano titanium dioxide slurry oil prepared by pre-dispersing the nano titanium dioxide in grease becomes a popular cosmetic raw material.
However, in the existing preparation method, in order to increase the powder content of the slurry oil, the viscosity of the prepared slurry oil is often higher, and in order to reduce the viscosity, a viscosity reducer is required to be added, and meanwhile, the problems of easy bonding, precipitation and the like are also caused, so that a plurality of auxiliary agents are required to be additionally added for solving the problems of bonding, precipitation and the like, the components of the slurry oil are complicated, and a plurality of troubles and unnecessary limitations are caused to the production of subsequent downstream products. Therefore, the nano titanium dioxide slurry produced by the prior art cannot be obtained by high powder content and low viscosity, and the components are simple and are not easy to adhere and precipitate.
Disclosure of Invention
Based on the above, it is necessary to provide a nano titanium dioxide slurry oil with high powder content, low viscosity, simple components and difficult adhesion and precipitation, and a preparation method and application thereof.
The invention provides a nano titanium dioxide slurry oil, which comprises the following components: grease, modified nano titanium dioxide and free PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane; the modified nano titanium dioxide is formed by depositing silicon dioxide on the surface,
Nanometer titania of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane.
In one embodiment, the modified nano titanium dioxide is used in an amount of 40-55% of the mass of the nano titanium dioxide slurry oil.
In one embodiment, the free PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is used in an amount of 0.5 to 5 percent of the mass of the nano-titania slurry oil.
In one embodiment, the particle size of the dispersoids in the nano titanium dioxide slurry oil is 40nm to 60nm.
In one embodiment, the grease is at least one of cyclopentadimethicone and dimethicone.
In the nano titanium dioxide slurry oil, the surface of the nano titanium dioxide is coated with a layer of silicon dioxide protective film, so that the weather resistance of the nano titanium dioxide is improved, and the reactive active sites on the surface of the powder are increased, so that the surface of the powder is easier to be modified
A group; surface-modified
The group can effectively improve the lipophilicity of the nano titanium dioxide; meanwhile, the dispersing agent PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane which is directly added into the oil slurry in the past is modified to the surface of the nano titanium dioxide, so that the steric hindrance between nano titanium dioxide particles is effectively increased, the modified nano titanium dioxide is not easy to agglomerate in the oil slurry, and hard precipitation is not caused after long-time placement. The nano titanium dioxide slurry oil provided by the invention has high powder content and low viscosity, can be placed for a long time without hardening and precipitation without adding an additive with high dosage and complex components, has good stability and simple components, and has wider application prospects in the preparation of downstream products.
In another aspect of the invention, a preparation method of the nano titanium dioxide slurry oil is provided, which comprises the following steps:
a) Uniformly spraying a mixture of triethoxy octyl silane and PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane on the surface of the nano titanium dioxide with silicon dioxide deposited on the surface, and drying to obtain the modified nano titanium dioxide;
b) Mixing and grinding the modified nano titanium dioxide, the free PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane and the grease to obtain the nano titanium dioxide slurry oil.
In one embodiment, the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane in step a) is used in an amount of 3-8% of the mass of the modified nano-titania.
In one embodiment, the amount of triethoxy octyl silane used in step a) is 0.5 to 10% of the mass of the modified nano titanium dioxide.
In one embodiment, the temperature of the drying in step a) is 100 ℃ to 120 ℃ and the drying time is 2.5 to 3.5 hours.
The invention also provides application of the nano titanium dioxide slurry oil in preparation of cosmetics and/or skin care products.
Detailed Description
In order that the invention may be readily understood, a more particular description of the invention will be rendered by reference to specific embodiments that are illustrated in the appended drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise. In the description of the present invention, the meaning of "several" means at least one, such as one, two, etc., unless specifically defined otherwise.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The invention provides a nano titanium dioxide slurry oil, which comprises the following components: grease, modified nano titanium dioxide and free PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane; the modified nano titanium dioxide is formed by depositing silicon dioxide on the surface,
Nanometer titania of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane.
In the present invention, the "free PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane" is relative to the portion of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane surface deposited on the surface of nano-titanium dioxide, which is not coated on the surface of nano-titanium dioxide, but is directly dispersed in grease to be used as a dispersing agent.
In a specific example, the amount of the modified nano titanium dioxide is 40% -55% of the mass of the nano titanium dioxide slurry oil, and preferably, the amount of the modified nano titanium dioxide is 43% -53% of the mass of the nano titanium dioxide slurry oil. The powder content in the nano titanium dioxide slurry oil is maintained in a preset range, so that the slurry oil has better stability and lower viscosity under the premise of reaching the highest powder content as much as possible, and the storage and use costs are lower.
In a specific example, the free PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is used in an amount of 0.5% -5% of the mass of the nano-titania slurry, preferably, the free PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is used in an amount of 2% -3% of the mass of the nano-titania slurry. The free PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane in the slurry oil can shield the polar groups on the surface of the nano titanium dioxide in a short time, increase the lipophilicity of the titanium dioxide and achieve the effect of instant viscosity reduction, so that the reasonable PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane dosage in the slurry oil can enable the nano titanium dioxide slurry oil of the invention to have high powder content and low viscosity.
In a specific example, the particle size of the dispersoid in the nano titanium dioxide slurry oil is 40nm to 60nm, preferably, the particle size of the dispersoid is 45nm to 55nm. The proper dispersoid particle size can lead the slurry oil dispersion system to have better stability and lower viscosity, and lead the downstream cosmetic product finished by subsequent processing to have better use feeling and efficacy.
In a specific example, the grease is at least one of cyclopentadimethicone and dimethicone.
In the nano titanium dioxide slurry oil, the surface of the nano titanium dioxide is coated with a layer of silicon dioxide protective film, so that the weather resistance of the nano titanium dioxide is improved, and the reactive active sites on the surface of the powder are increased, so that the surface of the powder is easier to be modified
A group; surface-modified
The group can effectively improve the lipophilicity of the nano titanium dioxide; meanwhile, the traditional dispersing agent PEG-9 polydimethylsiloxane in the oil slurry system is innovatively modified to the surface of nano titanium dioxide, so that the steric hindrance between nano titanium dioxide particles is effectively increased, the modified nano titanium dioxide is not easy to agglomerate and not hard to precipitate after being placed for a long time, a treatment idea which is different from the traditional treatment idea that the viscosity is reduced or the stability is improved by adding complex auxiliary agents or increasing the dosage of the auxiliary agents in the system is provided, the technical prejudice is overcome, the nano titanium dioxide oil slurry has low viscosity while having high powder content, and the nano titanium dioxide oil slurry can be placed for a long time without hard precipitation without adding the auxiliary agents with high dosage and complex components in the oil slurry, so that the stability of the oil slurry is effectively improved, and the components are simple, so that the nano titanium dioxide oil slurry has wider application prospect in the preparation of downstream products.
In another aspect of the invention, a preparation method of the nano titanium dioxide slurry oil is provided, which comprises the following steps:
a) Uniformly spraying a mixture of triethoxy octyl silane and PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane on the surface of the nano titanium dioxide with silicon dioxide deposited on the surface, and drying to obtain modified nano titanium dioxide;
alternatively, the manner of depositing silica on the nano titania may be: mixing nano titanium dioxide and silicate in a solvent, and then adjusting the pH to 6.5-8 to enable silicon dioxide to be deposited on the surface of the nano titanium dioxide, wherein the silicate can be selected from sodium silicate, potassium silicate and the like; optionally, the silicate is 0.1-10% of the nano titanium dioxide by mass, preferably, the silicate is 0.5-5% of the nano titanium dioxide by mass; the silica coating is carried out on the surface of the nano titanium dioxide, so that the nano titanium dioxide and surrounding medium can generate a barrier, the photochemical activity of the nano titanium dioxide is reduced, the light resistance of the nano titanium dioxide is improved, the nano titanium dioxide can be stably and nondegradable in the storage, transportation and subsequent production processes of downstream products, the chalk resistance of the nano titanium dioxide is primarily improved, and the reactive sites are increased. The silicate dosage is controlled in a proper range, so that the inorganic coating of the nano titanium dioxide is complete, and meanwhile, the silicon dioxide coated on the surface of the titanium dioxide is limited, so that the excessive uncoated silicon dioxide is avoided being formed due to the proper dosage, and the subsequent impurity removing procedure is complicated.
b) Mixing and grinding the modified nano titanium dioxide, the free PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane and the grease to obtain the nano titanium dioxide slurry oil.
In a specific example, the amount of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane in step a) is 3-8% of the mass of the modified nano-titania, preferably, the amount of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is 4-6% of the mass of the modified nano-titania. PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is a common dispersing agent used in the preparation of raw material slurry oil for cosmetics, and is used for reducing the viscosity of a slurry oil system, so that if the powder content of the slurry oil system is too high, the dosage of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane must be increased accordingly, however, the viscosity of the system can be effectively reduced due to the large amount of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane, but the problem of hard precipitation of slurry oil can not be solved, and after long-time placement, the system is easy to harden and precipitate, so that the slurry oil prepared by the conventional titanium dioxide slurry oil preparation method is often not high in powder content and low in viscosity, the stability of the system cannot be ensured even if a viscosity reducer is added, and in order to ensure long-time stability, other auxiliary agents with complex components have to be added, so that the components of a final slurry oil product are complex, and the application of the final slurry oil product in the subsequent preparation of a downstream product cosmetic is limited to a great extent. According to the preparation method, a part of dispersing agent PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane used in the preparation of the oil slurry is separated, and is added together with an organic modifier in one step of organic coating to be modified to the surface of nano titanium dioxide, so that physical modification is carried out on the nano titanium dioxide, and the surface of the nano titanium dioxide is modified with the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane, so that the modified nano titanium dioxide is not easy to agglomerate in the oil slurry, and is not hard to precipitate after being placed for a long time, and therefore, the low viscosity of the oil slurry with high powder content is realized under the condition that the dosage of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is not increased and other complex component additives are not introduced. In the proper dosage range, the steric hindrance on the surface of the nano titanium dioxide can be effectively increased, the agglomeration and precipitation are prevented, and meanwhile, the grinding process in the subsequent slurry preparation is not influenced by excessive dosage.
In a specific example, the amount of triethoxyoctylsilane used in step a) is 0.5% -10% of the mass of the modified nano-titania. Preferably, the use amount of the triethoxy octyl silane is 2 to 7 percent of the mass of the modified nano titanium dioxide; triethoxy octyl silane is a long chain silane, and is an organic surface modifier commonly used in the cosmetic field; the surface of the nano titanium dioxide is of strong polarity, so that the dispersing effect is poor in a nonpolar organic system; after the triethoxy octyl silane is used for carrying out organic coating on the nano titanium dioxide, the modification on the nano titanium dioxide is realized, and the compatibility and the dispersibility of the nano titanium dioxide in an organic system are improved to a great extent. The usage amount of the triethoxy octyl silane is in a proper range, so that the surface of the nano titanium dioxide is completely coated, better dispersibility can be achieved in an organic system, and meanwhile, excessive usage amount is avoided, so that excessive residual of the unreacted triethoxy octyl silane exists on the surface of the nano titanium dioxide, and the purity of the product is reduced.
In a specific example, the temperature of the drying in step a) is 100-120 ℃ and the drying time is 2.5-3.5 hours.
The invention also provides application of the nano titanium dioxide slurry oil in preparation of cosmetics and/or skin care products.
Preferably, the cosmetic and/or skin care product has a sun protection function.
The present invention will be described in further detail with reference to specific examples and comparative examples. It will be appreciated that the apparatus and materials used in the examples below are more specific and in other embodiments may not be so limited, e.g., the manner of grinding may not be limited to sanding.
Example 1
Titanium dioxide modification:
uniformly mixing triethoxy octyl silane and PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of nano titanium dioxide with silicon dioxide deposited on the surface under stirring, and drying at 110 ℃ for 3 hours to obtain modified nano titanium dioxide; wherein the dosage of the triethoxy octyl silane is 6 percent of the mass of the nano titanium dioxide with the silicon dioxide deposited on the surface, and the dosage of the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is 3 percent of the nano titanium dioxide with the silicon dioxide deposited on the surface;
step b), preparing oil slurry:
mixing modified nano titanium dioxide, PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and then sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 47% of the slurry oil in mass percent, the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane accounts for 3.5% of the slurry oil in mass percent, and the balance is cyclopenta-dimethylsiloxane.
Example 2
Titanium dioxide modification:
uniformly mixing triethoxy octyl silane and PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of nano titanium dioxide with silicon dioxide deposited on the surface under stirring, and drying at 110 ℃ for 3 hours to obtain modified nano titanium dioxide; wherein the dosage of the triethoxy octyl silane is 6 percent of the mass of the nano titanium dioxide with the silicon dioxide deposited on the surface, and the dosage of the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is 4 percent of the nano titanium dioxide with the silicon dioxide deposited on the surface;
step b), preparing oil slurry:
mixing modified nano titanium dioxide, PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and then sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 47.5 percent of the mass of the slurry oil, the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane accounts for 3 percent of the mass of the slurry oil, and the balance is cyclopenta-dimethylsiloxane.
Example 3
Titanium dioxide modification:
uniformly mixing triethoxy octyl silane and PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of nano titanium dioxide with silicon dioxide deposited on the surface under stirring, and drying at 110 ℃ for 3 hours to obtain modified nano titanium dioxide; wherein the dosage of the triethoxy octyl silane is 6 percent of the mass of the nano titanium dioxide with the silicon dioxide deposited on the surface, and the dosage of the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is 5 percent of the nano titanium dioxide with the silicon dioxide deposited on the surface;
step b), preparing oil slurry:
mixing modified nano titanium dioxide, PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and then sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 48 percent of the mass of the slurry oil, the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane accounts for 2.5 percent of the mass of the slurry oil, and the balance is cyclopenta-dimethylsiloxane.
Example 4
Titanium dioxide modification:
uniformly mixing triethoxy octyl silane and PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of nano titanium dioxide with silicon dioxide deposited on the surface under stirring, and drying at 110 ℃ for 3 hours to obtain modified nano titanium dioxide; wherein the dosage of the triethoxy octyl silane is 6 percent of the mass of the nano titanium dioxide with the silicon dioxide deposited on the surface, and the dosage of the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is 6 percent of the nano titanium dioxide with the silicon dioxide deposited on the surface;
step b), preparing oil slurry:
mixing modified nano titanium dioxide, PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and then sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 48.5 percent of the mass of the slurry oil, the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane accounts for 2 percent of the mass of the slurry oil, and the balance is cyclopenta-dimethylsiloxane.
Example 5
Titanium dioxide modification:
uniformly mixing triethoxy octyl silane and PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of nano titanium dioxide with silicon dioxide deposited on the surface under stirring, and drying at 110 ℃ for 3 hours to obtain modified nano titanium dioxide; wherein the dosage of the triethoxy octyl silane is 6 percent of the mass of the nano titanium dioxide with the silicon dioxide deposited on the surface, and the dosage of the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is 8 percent of the nano titanium dioxide with the silicon dioxide deposited on the surface;
step b), preparing oil slurry:
mixing modified nano titanium dioxide, PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and then sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 49.5% of the slurry oil in mass percent, the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane accounts for 1% of the slurry oil in mass percent, and the balance is cyclopenta-dimethylsiloxane.
Example 6
Titanium dioxide modification:
uniformly mixing triethoxyoctylsilane and PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of nano titanium dioxide with silicon dioxide deposited on the surface under stirring, and drying at 120 ℃ for 2.5 hours to obtain modified nano titanium dioxide; wherein the dosage of the triethoxy octyl silane is 8 percent of the mass of the nano titanium dioxide with the silicon dioxide deposited on the surface, and the dosage of the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is 5 percent of the nano titanium dioxide with the silicon dioxide deposited on the surface;
step b), preparing oil slurry:
mixing modified nano titanium dioxide, PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane and polydimethylsiloxane, and then sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 48 percent of the mass of the slurry oil, the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane accounts for 2.5 percent of the mass of the slurry oil, and the rest is polydimethylsiloxane.
Comparative example 1
Titanium dioxide modification:
uniformly mixing triethoxy octyl silane and PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of nano titanium dioxide with silicon dioxide deposited on the surface under stirring, and drying at 110 ℃ for 3 hours to obtain modified nano titanium dioxide; wherein the dosage of the triethoxy octyl silane is 6 percent of the mass of the nano titanium dioxide with the silicon dioxide deposited on the surface, and the dosage of the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is 1 percent of the nano titanium dioxide with the silicon dioxide deposited on the surface;
step b), preparing oil slurry:
mixing modified nano titanium dioxide, PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and then sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 46% of the slurry oil in mass percent, the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane accounts for 4.5% of the slurry oil in mass percent, and the balance is cyclopenta-dimethylsiloxane.
Comparative example 2
Titanium dioxide modification:
uniformly mixing triethoxy octyl silane and PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of nano titanium dioxide with silicon dioxide deposited on the surface under stirring, and drying at 110 ℃ for 3 hours to obtain modified nano titanium dioxide; wherein the dosage of the triethoxy octyl silane is 6 percent of the mass of the nano titanium dioxide with the silicon dioxide deposited on the surface, and the dosage of the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is 10 percent of the nano titanium dioxide with the silicon dioxide deposited on the surface;
step b), preparing oil slurry:
mixing modified nano titanium dioxide, PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and then sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 50% of the slurry oil in mass percent, the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane accounts for 0.5% of the slurry oil in mass percent, and the balance is cyclopenta-dimethylsiloxane.
Comparative example 3
Titanium dioxide modification:
uniformly mixing triethoxy octyl silane and PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of nano titanium dioxide with silicon dioxide deposited on the surface under stirring, and drying at 110 ℃ for 3 hours to obtain modified nano titanium dioxide; wherein the dosage of the triethoxy octyl silane is 6 percent of the mass of the nano titanium dioxide with the silicon dioxide deposited on the surface, and the dosage of the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is 5 percent of the nano titanium dioxide with the silicon dioxide deposited on the surface;
step b), preparing oil slurry:
mixing the modified nano titanium dioxide and the cyclopentadimethicone, and then sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 48% of the slurry oil by mass, and the balance is cyclopenta-dimethicone.
Comparative example 4
Titanium dioxide modification:
spraying triethoxy octyl silane on the surface of the nano titanium dioxide with silicon dioxide deposited on the surface under stirring, and baking at 110 ℃ for 3 hours to obtain modified nano titanium dioxide; wherein the consumption of the triethoxy octyl silane is 6% of the mass of the nano titanium dioxide with the silicon dioxide deposited on the surface;
step b), preparing oil slurry:
mixing modified nano titanium dioxide, PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and then sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 45 percent of the mass of the slurry oil, the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane accounts for 3 percent of the mass of the slurry oil, and the balance is cyclopenta-dimethylsiloxane.
Comparative example 5
Titanium dioxide modification:
spraying triethoxy octyl silane on the surface of the nano titanium dioxide with silicon dioxide deposited on the surface under stirring, and baking at 110 ℃ for 3 hours to obtain modified nano titanium dioxide; wherein the consumption of the triethoxy octyl silane is 6% of the mass of the nano titanium dioxide with the silicon dioxide deposited on the surface;
step b), preparing oil slurry:
mixing modified nano titanium dioxide, PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and then sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 45 percent of the mass of the slurry oil, the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane accounts for 5 percent of the mass of the slurry oil, and the balance is cyclopenta-dimethylsiloxane.
Comparative example 6
Titanium dioxide modification:
spraying triethoxy octyl silane on the surface of the nano titanium dioxide with silicon dioxide deposited on the surface under stirring, and baking at 110 ℃ for 3 hours to obtain modified nano titanium dioxide; wherein the consumption of the triethoxy octyl silane is 6% of the mass of the nano titanium dioxide with the silicon dioxide deposited on the surface;
step b), preparing oil slurry:
mixing modified nano titanium dioxide, PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and then sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 45 percent of the mass of the slurry oil, the PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane accounts for 7 percent of the mass of the slurry oil, and the balance is cyclopenta-dimethylsiloxane.
TABLE 1
The characterization of each example and comparative example is shown in Table 1, using a viscometer model: brookfield dv2T. As can be seen from the data of examples 1 to 5 of Table 1, when the total amount of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is controlled to be constant (about 4.9% of the slurry mass), the amount of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane in step b) is gradually increased with the amount of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane in step a), and the amount of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane in step b) is gradually decreased with the amount of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane in step b), so that the viscosity of the slurry is gradually increased; as can be seen from comparative example 1 and comparative examples 4 to 6, when the amount of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane in step a) is too small or not, although the viscosity of the slurry can be reduced by adding PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane in step b), the slurry system starts to form hard precipitation in a short time, while as can be seen from comparative example 2, when the amount of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane in step a) is too large, the dispersibility of nano titanium dioxide is also affected, and particles with too large particle size appear in the slurry system, which affect the subsequent processing and production of downstream products. Therefore, only if parameters in each step are controlled within preset ranges, and the dosage of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane in the step a) and the step b) is reasonably regulated, the slurry oil with high powder content can be prepared, has moderate viscosity, and can not generate hardening and precipitation after being placed for a long time.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (7)
1. The nano titanium dioxide slurry oil is characterized by being prepared by the following steps:
a) Uniformly spraying a mixture of triethoxy octyl silane and PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane on the surface of the nano titanium dioxide with silicon dioxide deposited on the surface, and drying to obtain modified nano titanium dioxide; the consumption of the triethoxy octyl silane is 0.5-10% of the mass of the modified nano titanium dioxide; the dosage of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane in the modified nano titanium dioxide is 3% -8% of the mass of the modified nano titanium dioxide;
b) Mixing and grinding the modified nano titanium dioxide, free PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane and grease to obtain nano titanium dioxide slurry oil; the free PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is 0.5% -5% of the mass of the nano titanium dioxide slurry oil; the dosage of the modified nano titanium dioxide is 40% -55% of the mass of the nano titanium dioxide slurry oil; the grease is at least one of cyclopentadimethicone and dimethicone.
2. The nano titanium dioxide slurry oil according to claim 1, wherein the particle size of the dispersoid in the nano titanium dioxide slurry oil is 40nm to 60nm.
3. The method for preparing the nano titanium dioxide slurry oil according to any one of claims 1 to 2, which is characterized by comprising the following steps:
a) Uniformly spraying a mixture of triethoxy octyl silane and PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane on the surface of the nano titanium dioxide with silicon dioxide deposited on the surface, and drying to obtain modified nano titanium dioxide; the dosage of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane in the modified nano titanium dioxide is 3% -8% of the mass of the modified nano titanium dioxide; the consumption of the triethoxy octyl silane is 0.5-10% of the mass of the modified nano titanium dioxide; b) Mixing and grinding the modified nano titanium dioxide, free PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane and grease to obtain nano titanium dioxide slurry oil; the free PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane is 0.5% -5% of the mass of the nano titanium dioxide slurry oil; the dosage of the modified nano titanium dioxide is 40% -55% of the mass of the nano titanium dioxide slurry oil; the grease is at least one of cyclopentadimethicone and dimethicone.
4. The method of claim 3, further comprising the step of depositing silica on the nano titania before step a), wherein the step of depositing silica on the nano titania comprises mixing the nano titania with silicate in a solvent and then adjusting the pH to 6.5-8 to deposit silica on the surface of the nano titania.
5. The method of claim 4, wherein the silicate is sodium silicate or potassium silicate; the silicate consumption is 0.1% -10% of the nano titanium dioxide mass.
6. The method according to any one of claims 3 to 5, wherein the temperature of the drying in step a) is 100 ℃ to 120 ℃, and the drying time is 2.5 to 3.5 hours.
7. The use of a nano titanium dioxide slurry oil according to any one of claims 1-2 in cosmetic preparation.
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