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Method for preparing Nano sol as ultraviolet protective agent

A technology of UV protective agent and nano-sol, which is applied in the direction of skin care preparations, cosmetic preparations, chemical instruments and methods, etc., can solve the problems of limiting the application field of UV protective agents, weak adhesion, oxidative corrosion, etc., and achieve Avoid rapid grain growth, strong adhesion, and good crystallization

Active Publication Date: 2009-09-09
GUANGDONG INST OF ECO ENVIRONMENT & SOIL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of rutile UV protective agent is also involved in many Chinese patents, such as patent 01126703.8, 200380110926.6, 200510111204.3 etc. have introduced the preparation method of rutile powder, but they have following shortcoming: (1) they all have under the radiation of ultraviolet light Strong photocatalytic activity, which will cause oxidative corrosion to substrates, especially organic materials; (2) They are usually used as pigments, and this white material usually cannot be used on substrates that require clean or colored surfaces. This also greatly limits its application field as a UV protective agent; (3) the prepared powder needs to be dispersed with a dispersant before it can be used, increasing the cost, and its adhesion is weak
But there is also a problem, that is, how to powder CeO 2 Dispersion for easy spraying or coating, and improve its adhesion

Method used

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  • Method for preparing Nano sol as ultraviolet protective agent
  • Method for preparing Nano sol as ultraviolet protective agent
  • Method for preparing Nano sol as ultraviolet protective agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1. Preparation of high-purity rutile sol with titanium tetrachloride as a precursor

[0030] Measure 50ml of titanium tetrachloride in a separatory funnel, add dropwise to 200ml of water in an ice-water bath, after the dropwise addition, stir for 1 hour; prepare 3L of ammonia water with a concentration of 2M. Add the titanium tetrachloride solution dropwise into the ammonia solution, and after the precipitation is fully reacted, adjust the pH to 10, stir for 4 hours, filter and wash until no chlorine ions are detected (tested by dropping 1.0M silver nitrate solution) ), then mix the filter cake with water according to the required preparation concentration, add 10% nitric acid, adjust the pH to 1.2, stir at room temperature for 4 hours, and then heat and stir in a 60°C water bath for 24 hours to obtain a uniform and stable rutile sol .

Embodiment 2

[0031] Example 2. Preparation of cerium dioxide sol with cerium nitrate as precursor

[0032] Accurately weigh 50 grams of cerium nitrate in 300ml of pure water, mix well, fully stir and dissolve, after cooling, add dropwise to 4M ammonia water, after fully reacting and precipitating, adjust the pH to 11, stir for 4 hours, filter, wash and precipitate until nothing Nitrate ions, and then mix the filter cake with water according to the required preparation concentration, add 10% nitric acid, adjust the pH to 1.5, stir at room temperature for 6 hours, and then heat and stir in a 70°C water bath for more than 20 hours to obtain a coarse sol , cooled immediately, and impurity ions were removed by means of nanofiltration or dialysis to obtain a stable yellow transparent ceria sol.

Embodiment 3

[0033] Example 3. Crystal structure (XRD) of rutile sol and ceria sol

[0034] Dry the rutile sol and ceria sol at 65°C for more than 12 hours, and grind them in an agate mortar to obtain powders. The XRD test results are as follows: figure 1 and figure 2 . Depend on figure 1 It can be seen that the XRD pattern is a rutile titanium dioxide structure (compared to JCPDS-0551), and several main diffraction peaks correspond to (110), (101), (111) and (211) crystal planes of rutile respectively. Depend on figure 2 It can be seen that the boundary of the spectrum is clear and the crystallization is in good condition, and several main diffraction peaks correspond to (111), (200), (220) and (311) crystal planes of ceria with a cristobalite structure respectively. The main peaks of both rutile (110) and ceria (111) are obviously broadened, indicating that they have a small grain size. The results show that the preparation method can successfully prepare nanocrystalline sols with...

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Abstract

The invention discloses a preparation method of a nano sol that can be used as an ultraviolet protective agent, which comprises (1) hydrolysis precipitation: adding an inorganic cerium salt or an inorganic titanium salt dropwise into water in an ice-water bath, stirring continuously, until the dropwise addition is complete , continue to stir, and obtain the solution after cooling; add the solution dropwise to the lye, and ensure that the pH of the lye after the dropwise addition is greater than 9, continue to stir; (2) filter and wash: filter, wash and precipitate to no impurity ions; (3) Degelization and crystallization: Add inorganic acid dropwise to the precipitate to adjust the pH to 0.1-2.0; after adding the acid, continue to stir at room temperature for more than 2 hours; then heat and stir in a water bath at 40-90°C for more than 3 hours , to obtain rutile sol or ceria sol that can be used as an ultraviolet protective agent. The nano-sol has the characteristics of strong ultraviolet shielding ability, low ultraviolet photocatalytic activity, strong adhesion, small particle size, and does not change the background color of the substrate.

Description

technical field [0001] The invention relates to the technical field of nano sol, in particular to a preparation method of nano sol which can be used as an ultraviolet protective agent. Background technique [0002] For a long time, oxides of zinc and titanium (such as ZnO, TiO 2 ) has always been the main compound as an inorganic anti-ultraviolet agent. In recent years, there have been some related literature reports, such as in ColloidInterf.Sci.300(2006)111, Colloid Polym.Sci.284(2006)422 and so on. Because of its strong UV shielding ability, low price and relatively weak photocatalytic activity compared with anatase, rutile occupies an important position in the application field of UV protection agent. The preparation method of rutile UV protective agent is also involved in many Chinese patents, such as patent 01126703.8, 200380110926.6, 200510111204.3 etc. have introduced the preparation method of rutile powder, but they have following shortcoming: (1) they all have un...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/053C01F17/00A61K8/19A61K8/29A61Q17/04
Inventor 刘同旭李芳柏刘新铭
Owner GUANGDONG INST OF ECO ENVIRONMENT & SOIL SCI