阅读说明：本技术 纳米二氧化钛油浆及其制备方法与应用 (Nano titanium dioxide slurry oil and preparation method and application thereof ) 是由 秦纪华 陈宗乐 谢旭 亢荣敏 于 2020-11-30 设计创作，主要内容包括：本发明涉及化妆品领域,特别是涉及一种纳米二氧化钛油浆及其制备方法与应用。本发明中纳米二氧化钛表面的二氧化硅保护膜能提高纳米二氧化钛的耐候性,同时增加了粉末表面的反应活性位点,使粉末表面更容易被修饰其他改性基团；表面修饰的基团能有效提高纳米二氧化钛的亲油性；表面修饰的PEG-9聚二甲基硅氧乙基聚二甲基硅氧烷使得改性后的纳米二氧化钛颗粒空间位阻增大,不易发生团聚。本发明的纳米二氧化钛油浆在具备高粉含量的同时能具备低粘度,油浆中无需加入高用量和成分复杂的助剂就能实现长时间放置而不结硬沉淀,油浆的稳定性好,且成分简单,在下游产品的制备中具有更广阔的应用前景。(The invention relates to the field of cosmetics, in particular to nano titanium dioxide oil slurry and a preparation method and application thereof. The silicon dioxide protective film on the surface of the nano titanium dioxide can improve the weather resistance of the nano titanium dioxide, and simultaneously increases the reactive sites on the surface of the powder, so that the surface of the powder is easier to be modified by other modified groups; surface modified)

1. The nanometer titanium dioxide slurry oil is characterized by comprising the following components: oil and fat, modifiedNanometer titanium dioxide and free PEG-9 polydimethylsiloxyethyl polydimethylsiloxane; the modified nano titanium dioxide is prepared by depositing silicon dioxide on the surface,And PEG-9 polydimethylsiloxyethyl polydimethylsiloxane.

2. The nano titanium dioxide slurry oil according to claim 1, wherein the amount of the modified nano titanium dioxide is 40-55% of the mass of the nano titanium dioxide slurry oil.

3. The nano titanium dioxide slurry oil according to claim 1, wherein the amount of the free PEG-9 polydimethylsiloxyethyl polydimethylsiloxane is 0.5-5% of the mass of the nano titanium dioxide slurry oil.

4. The nano titanium dioxide slurry oil according to any one of claims 1 to 3, wherein the particle size of dispersoids in the nano titanium dioxide slurry oil is 40nm to 60 nm.

5. The nano titanium dioxide slurry oil according to any one of claims 1 to 3, wherein the grease is at least one of cyclopentadimethylsiloxane and polydimethylsiloxane.

6. The preparation method of the nano titanium dioxide slurry oil according to any one of claims 1 to 5, characterized by comprising the following steps:

a) uniformly spraying a mixture of triethoxyoctylsilane and PEG-9 polydimethylsiloxyethyl 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 dimethyl silicone ethyl dimethyl silicone and the grease to obtain the nano titanium dioxide oil slurry.

7. The preparation method according to claim 6, wherein the amount of PEG-9 polydimethylsiloxyethyl polydimethylsiloxane in the step a) is 3-8% of the mass of the modified nano titanium dioxide.

8. The preparation method of claim 6, wherein the amount of the triethoxyoctylsilane used in the step a) is 0.5-10% of the mass of the modified nano titanium dioxide.

9. The preparation method according to any one of claims 6 to 8, wherein the drying temperature in step a) is 100 ℃ to 120 ℃, and the drying time is 2.5 to 3.5 hours.

10. Use of the nano titanium dioxide slurry oil according to any one of claims 1 to 5 in the preparation of cosmetics and/or skin care products.

Technical Field

The invention relates to the field of cosmetics, in particular to nano titanium dioxide oil slurry and a preparation method and application thereof.

Background

The nano titanium dioxide has the functions of absorbing and reflecting ultraviolet rays, and is one of widely used physical sun-screening agents. However, because the nano titanium dioxide has a large specific surface area and is easy to agglomerate to influence the use, the nano titanium dioxide oil slurry prepared by pre-dispersing the nano titanium dioxide in the oil becomes a more and more popular cosmetic raw material.

However, in the existing preparation method, in order to increase the powder content of the slurry, the viscosity of the prepared slurry is often too high, in order to reduce the viscosity, a viscosity reducer has to be added, and meanwhile, the problems of easy adhesion, easy precipitation and the like exist, so that a plurality of auxiliary agents are required to be additionally added for solving the problems of adhesion, precipitation and the like, which causes the components of the slurry to be complex, and causes a plurality of troubles and unnecessary limitations for the production of subsequent downstream products. Therefore, the nano titanium dioxide slurry produced by the prior art cannot meet the requirements of high powder content and low viscosity, and has simple components and difficult adhesion and precipitation.

Disclosure of Invention

Based on the above, there is a need to provide a nano titanium dioxide slurry oil with high powder content, low viscosity, simple components and less tendency to caking 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 polydimethylsiloxyethyl polydimethylsiloxane; the modified nano titanium dioxide is prepared by depositing silicon dioxide on the surface,And PEG-9 polydimethylsiloxyethyl polydimethylsiloxane.

In one embodiment, the dosage of the modified nano titanium dioxide is 40-55% of the mass of the nano titanium dioxide slurry oil.

In one embodiment, the amount of the free PEG-9 polydimethylsiloxyethyl polydimethylsiloxane is 0.5-5% of the mass of the nano titanium dioxide slurry.

In one embodiment, the particle size of the dispersoid in the nano titanium dioxide slurry oil is 40 nm-60 nm.

In one embodiment, the grease is at least one of cyclopentadimethylsiloxane and polydimethylsiloxane.

In the nano titanium dioxide slurry, 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 simultaneously, the reactive sites on the surface of the powder are increased, so that the surface of the powder is easier to modifyA group; surface modifiedThe group can effectively improve the lipophilicity of the nano titanium dioxide; meanwhile, the dispersing agent PEG-9 dimethyl silica ethyl dimethyl silicone which is directly added into the oil slurry in the past is modified on 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 the modified nano titanium dioxide can not be hardened and precipitated after being placed for a long time. The nano titanium dioxide slurry oil has high powder content and low viscosity, can be stored for a long time without hardening and precipitating without adding an additive with high dosage and complex components, has good stability and simple components, and has wider application prospect in the preparation of downstream products.

In another aspect of the present invention, a preparation method of the aforementioned nano titanium dioxide slurry oil is provided, which includes the following steps:

a) uniformly spraying a mixture of triethoxyoctylsilane and PEG-9 polydimethylsiloxyethyl 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 dimethyl silicone ethyl dimethyl silicone and the grease to obtain the nano titanium dioxide oil slurry.

In one embodiment, the amount of the PEG-9 polydimethylsiloxyethyl polydimethylsiloxane in the step a) is 3 to 8 percent of the mass of the modified nano titanium dioxide.

In one embodiment, the amount of the triethoxyoctylsilane used in the step a) is 0.5-10% of the mass of the modified nano titanium dioxide.

In one embodiment, the drying temperature in the step a) is 100-120 ℃, and the drying time is 2.5-3.5 hours.

The invention also provides an application of the nano titanium dioxide oil slurry in preparation of cosmetics and/or skin care products.

Detailed Description

In order that the invention may be more fully understood, reference will now be made to the accompanying examples. 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 "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the invention, "a plurality" means at least two, e.g., two, three, etc., unless explicitly specified otherwise. In the description of the present invention, "a plurality" means at least one, e.g., one, two, etc., unless specifically limited 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 in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" 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 polydimethylsiloxyethyl polydimethylsiloxane; the modified nano titanium dioxide is prepared by depositing silicon dioxide on the surface,And PEG-9 polydimethylsiloxyethyl polydimethylsiloxane.

In the present invention, the "free PEG-9 dimethiconoethyl polydimethylsiloxane" is relative to the PEG-9 dimethiconoethyl polydimethylsiloxane deposited on the surface of the nano titanium dioxide, and is not coated on the surface of the nano titanium dioxide, but is directly dispersed in the grease to be used as a dispersant.

In a specific example, the amount of the modified nano titanium dioxide is 40 to 55 percent of the mass of the nano titanium dioxide slurry oil, and preferably, the amount of the modified nano titanium dioxide is 43 to 53 percent of the mass of the nano titanium dioxide slurry oil. The powder content in the nano titanium dioxide slurry oil is maintained within a preset range, so that the slurry oil has better stability and lower viscosity on the premise of reaching the highest powder content, and the storage and use cost is lower.

In a specific example, the amount of the free PEG-9 polydimethylsiloxyethyl polydimethylsiloxane is 0.5 to 5 percent of the mass of the nano titanium dioxide oil slurry, and preferably, the amount of the free PEG-9 polydimethylsiloxyethyl polydimethylsiloxane is 2 to 3 percent of the mass of the nano titanium dioxide oil slurry. Free PEG-9 dimethyl silica ethyl dimethyl silicone in the oil slurry can shield 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 amount of the PEG-9 dimethyl silica ethyl dimethyl silicone in the oil slurry enables the nano titanium dioxide oil slurry to have both high powder content and low viscosity.

In one specific example, the particle size of the dispersoid in the nano titanium dioxide slurry oil is 40nm to 60nm, and preferably, the particle size of the dispersoid is 45nm to 55 nm. The appropriate particle size of the dispersoid can enable the oil slurry dispersion to have better stability and lower viscosity, and enable downstream cosmetic products after subsequent processing to have better use feeling and efficacy.

In a specific example, the grease is at least one of cyclopentadimethylsiloxane and polydimethylsiloxane.

In the nano titanium dioxide slurry, 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 simultaneously, the reactive sites on the surface of the powder are increased, so that the surface of the powder is easier to modifyA group; surface modifiedThe group can effectively improve the lipophilicity of the nano titanium dioxide; meanwhile, a dispersing agent PEG-9 dimethyl silica ethyl dimethyl polysiloxane which is only used in an oil slurry system in the past is innovatively modified on the surface of the nano titanium dioxide, so that the steric hindrance among nano titanium dioxide particles is effectively increased, the modified nano titanium dioxide is not easy to agglomerate in the oil slurry, and the nano titanium dioxide can not be hardened and precipitated after being placed for a long timeThe stability of the oil slurry is improved, and the components are simple, so that the oil slurry has a wider application prospect in the preparation of downstream products.

In another aspect of the present invention, a preparation method of the aforementioned nano titanium dioxide slurry oil is provided, which includes the following steps:

a) uniformly spraying a mixture of triethoxyoctylsilane and PEG-9 polydimethylsiloxyethyl 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 the silicon dioxide on the nano titanium dioxide can be as follows: mixing nano titanium dioxide and silicate in a solvent, and adjusting the pH value 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 amount of the silicate is 0.1-10% of the mass of the nano titanium dioxide, and preferably, the amount of the silicate is 0.5-5% of the mass of the nano titanium dioxide; the silicon dioxide coating is carried out on the surface of the nano titanium dioxide, so that the nano titanium dioxide and surrounding media 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 stably exist in the processes of storage, transportation and subsequent production of downstream products without decomposition, the powdering resistance of the nano titanium dioxide is preliminarily improved, and reaction active 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, because the silicon dioxide coated on the surface of the titanium dioxide is limited, the proper dosage also avoids the formation of redundant uncoated silicon dioxide, so that the subsequent impurity removal procedure is complicated.

b) Mixing the modified nano titanium dioxide, free PEG-9 dimethyl silica ethyl dimethyl silicone and grease, and grinding to obtain nano titanium dioxide slurry oil.

In a specific example, the amount of PEG-9 polydimethylsiloxyethyl polydimethylsiloxane in the step a) is 3 to 8 percent of the mass of the modified nano titanium dioxide, and preferably, the amount of PEG-9 polydimethylsiloxyethyl polydimethylsiloxane is 4 to 6 percent of the mass of the modified nano titanium dioxide. PEG-9 dimethyl silica ethyl dimethyl silicone is a dispersing agent commonly used in the preparation of cosmetic raw material oil slurry, and is used for reducing the viscosity of an oil slurry system, so if the powder content of the oil slurry system is too high, the using amount of PEG-9 dimethyl silica ethyl dimethyl silicone must be increased, however, although the use amount of PEG-9 dimethyl silica ethyl dimethyl silicone can effectively reduce the viscosity of the system, the problem that the powder slurry generates hard precipitate cannot be solved, after the powder slurry is placed for a long time, the system is easy to be hardened and precipitated, therefore, the oil slurry prepared in the existing titanium dioxide oil slurry preparation method often cannot have both high powder content and low viscosity, even if a viscosity reducer is added, the stability of the system cannot be ensured, in order to ensure the long-time stability, other auxiliary agents with complex components have to be added, resulting in a complex composition of the final slurry product, which greatly limits its use in subsequent downstream product cosmetic preparations. The application innovatively divides a dispersant PEG-9 dimethyl silica ethyl dimethyl silicone used in the past oil slurry preparation into a part, the part is added with an organic modifier in one step of organic coating to modify the surface of nano titanium dioxide, and the nano titanium dioxide is physically modified, because the steric hindrance between nano titanium dioxide particles of PEG-9 dimethyl silica ethyl dimethyl silicone modified on the surface is increased, the modified nano titanium dioxide is not easy to agglomerate in the oil slurry, and the nano titanium dioxide can not be hardened and precipitated after being placed for a long time, thereby realizing the low viscosity of the oil slurry with high powder content under the condition that the use amount of the PEG-9 dimethyl silica ethyl dimethyl silicone is not increased and other complex component auxiliaries are not introduced, simultaneously, the oil slurry has good stability, can not be hardened and precipitated after being placed for a long time, and because the components are simple, the use of downstream products also reduces unnecessary restrictions. Within a proper dosage range, the steric hindrance of the surface of the nano titanium dioxide can be effectively increased, the agglomeration and the precipitation can be prevented, and meanwhile, the grinding process in the subsequent oil slurry preparation can not be influenced due to excessive dosage.

In a specific example, the amount of the triethoxyoctylsilane in the step a) is 0.5-10% of the mass of the modified nano titanium dioxide. Preferably, the amount of the triethoxyoctylsilane is 2 to 7 percent of the mass of the modified nano titanium dioxide; triethoxyoctylsilane is a long-chain silane, and is an organic surface modifier commonly used in the field of cosmetics; the surface of the nano titanium dioxide is strong in polarity, so that the nano titanium dioxide has poor dispersion effect in a nonpolar organism system; the triethoxyoctylsilane is used for organically coating the nano titanium dioxide, so that the nano titanium dioxide is modified, and the compatibility and the dispersibility of the nano titanium dioxide in an organic system are improved to a great extent. The dosage of the triethoxyoctylsilane is in a proper range, so that the surface of the nano titanium dioxide is completely coated organically, the nano titanium dioxide has better dispersibility in an organic system, and simultaneously, the excessive consumption of the triethoxyoctylsilane can not cause the excessive unreacted residue of the triethoxyoctylsilane on the surface of the nano titanium dioxide, thereby reducing the purity of the product.

In a specific example, the drying temperature in the step a) is 100-120 ℃, and the drying time is 2.5-3.5 hours.

The invention also provides an application of the nano titanium dioxide oil slurry in preparation of cosmetics and/or skin care products.

Preferably, the cosmetic and/or skin care product has a sunscreen function.

The present invention will be described in further detail with reference to specific examples and comparative examples. It is understood that the following examples are more specific to the apparatus and materials used, and in other embodiments, the invention is not limited thereto, e.g., the grinding means may not be limited to sanding.

Example 1

Step a) titanium dioxide modification:

uniformly mixing triethoxyoctylsilane and PEG-9 polydimethylsiloxyethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of the 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 triethoxyoctylsilane is 6 percent of the mass of the nano titanium dioxide with silicon dioxide deposited on the surface, and the dosage of the PEG-9 polydimethylsiloxyethyl polydimethylsiloxane is 3 percent of the nano titanium dioxide with silicon dioxide deposited on the surface;

step b) preparation of oil slurry:

mixing the modified nano titanium dioxide, PEG-9 polydimethylsiloxyethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 47 percent of the oil slurry by mass, the PEG-9 polydimethylsiloxyethyl polydimethylsiloxane accounts for 3.5 percent of the oil slurry by mass, and the rest is cyclopenta polydimethylsiloxane.

Example 2

Step a) titanium dioxide modification:

uniformly mixing triethoxyoctylsilane and PEG-9 polydimethylsiloxyethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of the 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 triethoxyoctylsilane is 6 percent of the mass of the nano titanium dioxide with silicon dioxide deposited on the surface, and the dosage of the PEG-9 polydimethylsiloxyethyl polydimethylsiloxane is 4 percent of the nano titanium dioxide with silicon dioxide deposited on the surface;

step b) preparation of oil slurry:

mixing the modified nano titanium dioxide, PEG-9 polydimethylsiloxyethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 47.5 percent of the oil slurry by mass, the PEG-9 polydimethylsiloxyethyl polydimethylsiloxane accounts for 3 percent of the oil slurry by mass, and the rest is cyclopenta polydimethylsiloxane.

Example 3

Step a) titanium dioxide modification:

uniformly mixing triethoxyoctylsilane and PEG-9 polydimethylsiloxyethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of the 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 triethoxyoctylsilane is 6 percent of the mass of the nano titanium dioxide with silicon dioxide deposited on the surface, and the dosage of the PEG-9 polydimethylsiloxyethyl polydimethylsiloxane is 5 percent of the nano titanium dioxide with silicon dioxide deposited on the surface;

step b) preparation of oil slurry:

mixing the modified nano titanium dioxide, PEG-9 polydimethylsiloxyethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 48 percent of the oil slurry by mass, the PEG-9 polydimethylsiloxyethyl polydimethylsiloxane accounts for 2.5 percent of the oil slurry by mass, and the rest is cyclopenta polydimethylsiloxane.

Example 4

Step a) titanium dioxide modification:

uniformly mixing triethoxyoctylsilane and PEG-9 polydimethylsiloxyethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of the 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 triethoxyoctylsilane 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 polydimethylsiloxyethyl polydimethylsiloxane is 6 percent of the nano titanium dioxide with the silicon dioxide deposited on the surface;

step b) preparation of oil slurry:

mixing the modified nano titanium dioxide, PEG-9 polydimethylsiloxyethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 48.5 percent of the oil slurry by mass, the PEG-9 polydimethylsiloxyethyl polydimethylsiloxane accounts for 2 percent of the oil slurry by mass, and the rest is cyclopenta polydimethylsiloxane.

Example 5

Step a) titanium dioxide modification:

uniformly mixing triethoxyoctylsilane and PEG-9 polydimethylsiloxyethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of the 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 triethoxyoctylsilane is 6 percent of the mass of the nano titanium dioxide with silicon dioxide deposited on the surface, and the dosage of the PEG-9 polydimethylsiloxyethyl polydimethylsiloxane is 8 percent of the nano titanium dioxide with silicon dioxide deposited on the surface;

step b) preparation of oil slurry:

mixing the modified nano titanium dioxide, PEG-9 polydimethylsiloxyethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 49.5 percent of the oil slurry by mass, the PEG-9 polydimethylsiloxyethyl polydimethylsiloxane accounts for 1 percent of the oil slurry by mass, and the rest is cyclopenta polydimethylsiloxane.

Example 6

Step a) titanium dioxide modification:

uniformly mixing triethoxyoctylsilane and PEG-9 polydimethylsiloxyethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of the nano titanium dioxide with silicon dioxide deposited on the surface under stirring, and drying for 2.5 hours at 120 ℃ to obtain modified nano titanium dioxide; wherein the dosage of the triethoxyoctylsilane accounts for 8% of the mass of the nano titanium dioxide with silicon dioxide deposited on the surface, and the dosage of the PEG-9 polydimethylsiloxyethyl polydimethylsiloxane accounts for 5% of the nano titanium dioxide with silicon dioxide deposited on the surface;

step b) preparation of oil slurry:

mixing the modified nano titanium dioxide, PEG-9 polydimethylsiloxyethyl polydimethylsiloxane and polydimethylsiloxane, and sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 48 percent of the oil slurry by mass, the PEG-9 polydimethylsiloxane accounts for 2.5 percent of the oil slurry by mass, and the rest part is the polydimethylsiloxane.

Comparative example 1

Step a) titanium dioxide modification:

uniformly mixing triethoxyoctylsilane and PEG-9 polydimethylsiloxyethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of the 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 triethoxyoctylsilane 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 polydimethylsiloxyethyl polydimethylsiloxane is 1 percent of the nano titanium dioxide with the silicon dioxide deposited on the surface;

step b) preparation of oil slurry:

mixing the modified nano titanium dioxide, PEG-9 polydimethylsiloxyethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 46 percent of the oil slurry by mass, the PEG-9 polydimethylsiloxyethyl polydimethylsiloxane accounts for 4.5 percent of the oil slurry by mass, and the rest is cyclopenta polydimethylsiloxane.

Comparative example 2

Step a) titanium dioxide modification:

uniformly mixing triethoxyoctylsilane and PEG-9 polydimethylsiloxyethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of the 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 triethoxyoctylsilane is 6 percent of the mass of the nano titanium dioxide with silicon dioxide deposited on the surface, and the dosage of the PEG-9 polydimethylsiloxyethyl polydimethylsiloxane is 10 percent of the nano titanium dioxide with silicon dioxide deposited on the surface;

step b) preparation of oil slurry:

mixing the modified nano titanium dioxide, PEG-9 polydimethylsiloxyethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 50 percent of the oil slurry by mass, the PEG-9 polydimethylsiloxyethyl polydimethylsiloxane accounts for 0.5 percent of the oil slurry by mass, and the rest is cyclopenta polydimethylsiloxane.

Comparative example 3

Step a) titanium dioxide modification:

uniformly mixing triethoxyoctylsilane and PEG-9 polydimethylsiloxyethyl polydimethylsiloxane to obtain a mixture, spraying the mixture on the surface of the 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 triethoxyoctylsilane is 6 percent of the mass of the nano titanium dioxide with silicon dioxide deposited on the surface, and the dosage of the PEG-9 polydimethylsiloxyethyl polydimethylsiloxane is 5 percent of the nano titanium dioxide with silicon dioxide deposited on the surface;

step b) preparation of oil slurry:

mixing the modified nano titanium dioxide and cyclopentadidimethyl siloxane, and sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 48% of the oil slurry by mass, and the rest is cyclopentadidimethyl siloxane.

Comparative example 4

Step a) titanium dioxide modification:

spraying triethoxyoctylsilane on the surface of the nano titanium dioxide with silicon dioxide deposited on the surface under stirring, and drying for 3 hours at 110 ℃ to obtain modified nano titanium dioxide; wherein the dosage of the triethoxyoctylsilane is 6 percent of the mass of the nano titanium dioxide with silicon dioxide deposited on the surface;

step b) preparation of oil slurry:

mixing the modified nano titanium dioxide, PEG-9 polydimethylsiloxyethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 45% of the oil slurry by mass, the PEG-9 polydimethylsiloxane accounts for 3% of the oil slurry by mass, and the rest is cyclopenta polydimethylsiloxane.

Comparative example 5

Step a) titanium dioxide modification:

spraying triethoxyoctylsilane on the surface of the nano titanium dioxide with silicon dioxide deposited on the surface under stirring, and drying for 3 hours at 110 ℃ to obtain modified nano titanium dioxide; wherein the dosage of the triethoxyoctylsilane is 6 percent of the mass of the nano titanium dioxide with silicon dioxide deposited on the surface;

step b) preparation of oil slurry:

mixing the modified nano titanium dioxide, PEG-9 polydimethylsiloxyethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 45% of the oil slurry by mass, the PEG-9 polydimethylsiloxane accounts for 5% of the oil slurry by mass, and the rest is cyclopenta polydimethylsiloxane.

Comparative example 6

Step a) titanium dioxide modification:

spraying triethoxyoctylsilane on the surface of the nano titanium dioxide with silicon dioxide deposited on the surface under stirring, and drying for 3 hours at 110 ℃ to obtain modified nano titanium dioxide; wherein the dosage of the triethoxyoctylsilane is 6 percent of the mass of the nano titanium dioxide with silicon dioxide deposited on the surface;

step b) preparation of oil slurry:

mixing the modified nano titanium dioxide, PEG-9 polydimethylsiloxyethyl polydimethylsiloxane and cyclopentadimethylsiloxane, and sanding to obtain nano titanium dioxide slurry oil; wherein the modified nano titanium dioxide accounts for 45% of the oil slurry by mass, the PEG-9 polydimethylsiloxane accounts for 7% of the oil slurry by mass, and the rest is cyclopenta polydimethylsiloxane.

TABLE 1

In Table 1, the characterization of each example and comparative example is done using a viscometer of the type: brookfield dv 2T. As can be seen from the data of examples 1 to 5 in Table 1, when the total amount of PEG-9 PDMS is controlled to be a certain amount (about 4.9% of the slurry), the amount used in step b) is reduced with the gradual increase of the amount used in step a), and therefore the viscosity of the slurry finally increases gradually, which indicates that the amount of PEG-9 PDMS in step b) has a direct effect on the viscosity of the slurry; as can be seen from comparative examples 1 and 4-6, when the amount of PEG-9 PDMS in step a) is too small or not, although the viscosity of the slurry can be reduced by adding PEG-9 PDMS in step b), the slurry system will begin to form hard precipitates in a short time, and as can be seen from comparative example 2, when the amount of PEG-9 PDMS in step a) is too large, the dispersibility of the nano titanium dioxide will be affected, and particles with too large particle size will appear in the slurry system, which will affect the processing and production of subsequent downstream products. Therefore, only by controlling the parameters in each step within the preset range and reasonably adjusting the dosage of PEG-9 polydimethylsiloxyethyl polydimethylsiloxane in the step a) and the step b), the oil slurry with high powder content can be prepared, has moderate viscosity and can not generate hardening precipitation after being placed for a long time.

The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.

The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.