Ultraviolet light absorber and preparation method thereof

Abstract

The invention relates to the technical field of ultraviolet light absorbers, in particular to an ultraviolet light absorber and a preparation method thereof. The invention provides an ultraviolet light absorber and a preparation method thereof, and the ultraviolet light absorber comprises the following components by weight: 20-30 parts of a sun-screening agent; 10 to 20 parts of an ester antioxidant; 5 to 15 parts of titanium dioxide nano particles; 0.5 to 1 part of an antioxidant; and 50-60 parts of a solvent. The prepared ultraviolet light absorber has the advantages of wide absorption wave band, high absorption efficiency and good weather resistance.

Description

Technical Field

[0001] The invention relates to the technical field of ultraviolet light absorbers, and in particular to an ultraviolet light absorber and a preparation method thereof. Background Art

[0002] Ultraviolet light absorbers are a class of compounds that can absorb ultraviolet light and convert its energy into harmless energy. They are widely used in plastics, coatings, cosmetics and other fields to protect materials from damage by ultraviolet light. However, existing ultraviolet light absorbers have problems such as narrow absorption band and poor weather resistance. Therefore, it is of great significance to develop an ultraviolet light absorber with excellent performance. Summary of the invention

[0003] In order to overcome at least one of the defects of the prior art, the present invention provides an ultraviolet light absorber and a preparation method thereof. The ultraviolet light absorber prepared by the present invention has a wide absorption band, high absorption efficiency and good weather resistance.

[0004] The technical solution adopted by the present invention to solve the problem is:

[0005] An ultraviolet light absorber, comprising the following components in parts by weight:

[0006] Sunscreen: 20-30 parts;

[0007] Ester antioxidant: 10-20 parts;

[0008] Titanium dioxide nanoparticles: 5-15 parts;

[0009] Antioxidant: 0.5-1 part;

[0010] Solvent: 50-60 parts.

[0011] Furthermore, the sunscreen agent is 2-hydroxy-4-methoxybenzophenone.

[0012] Furthermore, the antioxidant is butylated hydroxytoluene.

[0013] Furthermore, the solvent includes one or more of ethanol and ethyl acetate.

[0014] Furthermore, the ester antioxidant is 3,5-di-tert-butyl-4-hydroxyphenylpropionate.

[0015] By adopting the above scheme, 3,5-di-tert-butyl-4-hydroxyphenylpropionate plays a role in delaying oxidative degradation, has excellent antioxidant properties, can effectively capture and neutralize free radicals, and prevent the material from being degraded under the action of light, heat and oxygen.

[0016] The present invention also provides a method for preparing the ultraviolet light absorber, comprising the following steps:

[0017] S1. Preparation of precursor material: 20-30 parts of 2-hydroxy-4-methoxybenzophenone are placed in a reaction container; and 10-20 parts of an ester antioxidant are added to the reaction container and mixed thoroughly;

[0018] S2. Dispersion of nanoparticles: Dispersing 5-15 parts of titanium dioxide nanoparticles in 50-60 parts of solvent to ensure that the nanoparticles are fully and evenly dispersed in the solvent;

[0019] S3, initial mixing reaction: slowly adding the precursor material mixed in step S1 to the titanium dioxide nanoparticle solution dispersed in step S2, while keeping stirring;

[0020] S4, secondary mixing reaction: gradually add 0.5-1 part of antioxidant to the mixture in step S3, and continue stirring to ensure that all components are evenly mixed;

[0021] S5, solvent evaporation: transferring the solution in step S4 to an evaporation device to evaporate excess solvent until a dry UV absorber solid powder is obtained;

[0022] S6. Powder grinding: grinding the obtained UV absorber solid powder to obtain UV absorber powder.

[0023] Furthermore, in the step S2, an ultrasonic disperser is used for ultrasonic dispersion for 30-60 minutes.

[0024] By adopting the above scheme, an ultrasonic disperser is used to ensure that the titanium dioxide nanoparticles are fully and evenly dispersed in the solvent.

[0025] Furthermore, the stirring speed in step S3 is 300-500 rpm, and the stirring time in step S4 is 30-60 min.

[0026] By adopting the above scheme, the uniform mixing effect of each component is guaranteed.

[0027] Furthermore, the evaporation device in step S5 is a rotary evaporator, and rotary evaporation is performed at 50°C-70°C.

[0028] By adopting the above scheme, the excess solvent is evaporated by a rotary evaporator to obtain a dry ultraviolet light absorber solid powder.

[0029] Furthermore, the grinding in step S6 is performed using a ball mill and the grinding is performed for 2-4 hours.

[0030] By adopting the above scheme, fine powder of the ultraviolet light absorber is obtained by ball milling for 2-4 hours.

[0031] In summary, the ultraviolet light absorber and the preparation method thereof provided by the present invention have the following technical effects:

[0032] 1. The ultraviolet light absorber of the present invention has a wide absorption band, high absorption efficiency and good weather resistance;

[0033] 2. The ultraviolet light absorber of the present invention has good ultraviolet light absorption performance in the range of 200-400nm. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 A flow chart of the preparation method of an embodiment of the present invention. DETAILED DESCRIPTION

[0035] For better understanding and implementation, the technical solutions in the embodiments of the present invention will be clearly and completely described and discussed below in conjunction with the accompanying drawings of the present invention. Obviously, what is described here is only a part of the examples of the present invention, not all the examples. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0036] In order to facilitate the understanding of the embodiments of the present invention, the following will be further explained by taking specific embodiments as examples in conjunction with the drawings, and each embodiment does not constitute a limitation on the embodiments of the present invention.

[0037] In the description of the present invention, it should be noted that the terms "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside" and "outside" etc. indicate directions or positional relationships based on the directions or positional relationships shown in the accompanying drawings. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific direction, be constructed and operated in a specific direction. Therefore, they cannot be understood as limiting the present invention.

[0038] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used in the specification of the present invention herein are only for the purpose of describing specific embodiments and are not intended to limit the present invention.

[0039] See also Figure 1 , the present invention discloses an ultraviolet light absorber and a preparation method thereof: in parts by weight, it comprises the following components: sunscreen: 20-30 parts;

[0040] Ester antioxidant: 10-20 parts;

[0041] Titanium dioxide nanoparticles: 5-15 parts;

[0042] Antioxidant: 0.5-1 part;

[0043] Solvent: 50-60 parts.

[0044] Specifically, in parts by weight, the sunscreen in the ultraviolet light absorber disclosed in the present invention is 20-30 parts, wherein preferably, the weight of the sunscreen is 25 parts. In an embodiment of the present invention, the sunscreen is 2-hydroxy-4-methoxybenzophenone.

[0045] Specifically, in parts by weight, the ester antioxidant in the ultraviolet light absorber disclosed in the present invention is 10-20 parts, wherein preferably, the weight of the ester antioxidant is 15 parts. In an embodiment of the present invention, the ester antioxidant is 3,5-di-tert-butyl-4-hydroxyphenylpropionate.

[0046] Specifically, in parts by weight, the titanium dioxide nanoparticles in the ultraviolet light absorber disclosed in the present invention are 5-15 parts, wherein preferably, the weight of the titanium dioxide nanoparticles is 8 parts.

[0047] Specifically, the present invention discloses an ultraviolet light absorber in which the antioxidant is 0.5-1 part by weight, wherein preferably, the weight of the antioxidant is 0.75 parts. In an embodiment of the present invention, the antioxidant is butylated hydroxytoluene.

[0048] Specifically, the present invention discloses a UV absorber in which the solvent is 50-60 parts by weight, wherein preferably, the weight of the solvent is 55 parts, and in an embodiment of the present invention, the solvent is one or more of ethanol and ethyl acetate. When the solvent is ethanol and ethyl acetate, the total weight of ethanol and ethyl acetate is 50-60 parts.

[0049] The present invention also provides a method for preparing an ultraviolet light absorber, comprising the following steps:

[0050] S1. Preparation of precursor material: 20-30 parts of 2-hydroxy-4-methoxybenzophenone are placed in a reaction container; and 10-20 parts of an ester antioxidant are added to the reaction container and mixed thoroughly;

[0051] S2, dispersion of nanoparticles: 5-15 parts of titanium dioxide nanoparticles are dispersed in 50-60 parts of a solvent to ensure that the nanoparticles are fully and evenly dispersed in the solvent; wherein, in the step S2, an ultrasonic disperser is used for ultrasonic dispersion for 30-60 minutes to ensure that the titanium dioxide nanoparticles are fully and evenly dispersed in the solvent by the ultrasonic disperser;

[0052] S3, initial mixing reaction: slowly add the precursor material mixed in step S1 to the titanium dioxide nanoparticle solution dispersed in step S2, the stirring speed in step S3 is 300-500 rpm, and the stirring is maintained to ensure uniform mixing of the components.

[0053] S4, secondary mixing reaction: gradually add 0.5-1 part of antioxidant to the mixture in step S3, and continue stirring to ensure that the components are evenly mixed; the stirring time in step S4 is 30-60 minutes to ensure uniform stirring and mixing effect;

[0054] S5, solvent evaporation: transferring the solution in step S4 to an evaporation device, evaporating excess solvent until a dry ultraviolet light absorber solid powder is obtained; the evaporation device in step S5 is a rotary evaporator, and rotary evaporation is performed at 50° C.-70° C. The rotary evaporator evaporates excess solvent to obtain a dry ultraviolet light absorber solid powder;

[0055] S6, powder grinding: grinding the obtained UV absorber solid powder to obtain UV absorber powder; the grinding in step S6 is performed using a ball mill and grinding for 2-4 hours to obtain fine UV absorber powder.

[0056] In summary, the ultraviolet light absorber and the preparation method thereof provided by the present invention have the following technical effects:

[0057] 1. The ultraviolet light absorber of the present invention has a wide absorption band, high absorption efficiency and good weather resistance;

[0058] 2. The ultraviolet light absorber of the present invention has good ultraviolet light absorption performance in the range of 200-400nm.

[0059] Embodiment 1 of the present invention:

[0060] Take 20 kg of 2-hydroxy-4-methoxybenzophenone and place it in a reaction container, and add 10 kg of 3,5-di-tert-butyl-4-hydroxyphenylpropionate into the reaction container and mix thoroughly;

[0061] Disperse 5 kg of titanium dioxide nanoparticles in 50 kg of solution to ensure that the nanoparticles are fully and evenly dispersed in the solvent;

[0062] Slowly add the mixed 2-hydroxy-4-methoxybenzophenone and 3,5-di-tert-butyl-4-hydroxyphenylpropionate into the dispersed titanium dioxide nanoparticle solution while stirring;

[0063] 0.5 kg of butylated hydroxytoluene was added to the 2-hydroxy-4-methoxybenzophenone, 3,5-di-tert-butyl-4-hydroxyphenylpropionate and titanium dioxide nanoparticle solution, and stirring was continued to ensure that the components were evenly mixed;

[0064] The above solution is transferred to a rotary evaporator to evaporate excess solvent until dry ultraviolet light absorber solid powder is obtained, and then the ultraviolet light absorber solid powder is ground to obtain ultraviolet light absorber powder.

[0065] Embodiment 2 of the present invention:

[0066] Take 30 kg of 2-hydroxy-4-methoxybenzophenone and put it in a reaction container, and add 20 kg of 3,5-di-tert-butyl-4-hydroxyphenylpropionate into the reaction container and mix thoroughly;

[0067] Disperse 15 kg of titanium dioxide nanoparticles in 60 kg of solution to ensure that the nanoparticles are fully and evenly dispersed in the solvent;

[0068] Slowly add the mixed 2-hydroxy-4-methoxybenzophenone and 3,5-di-tert-butyl-4-hydroxyphenylpropionate into the dispersed titanium dioxide nanoparticle solution while stirring;

[0069] 1 kg of butylated hydroxytoluene was added to the 2-hydroxy-4-methoxybenzophenone, 3,5-di-tert-butyl-4-hydroxyphenylpropionate and titanium dioxide nanoparticle solution, and stirring was continued to ensure that the components were evenly mixed;

[0070] The above solution is transferred to a rotary evaporator to evaporate excess solvent until dry ultraviolet light absorber solid powder is obtained, and then the ultraviolet light absorber solid powder is ground to obtain ultraviolet light absorber powder.

[0071] Embodiment 3 of the present invention:

[0072] Take 25 kg of 2-hydroxy-4-methoxybenzophenone and place it in a reaction container, and add 15 kg of 3,5-di-tert-butyl-4-hydroxyphenylpropionate into the reaction container and mix thoroughly;

[0073] Disperse 8 kg of titanium dioxide nanoparticles in 55 kg of solution to ensure that the nanoparticles are fully and evenly dispersed in the solvent;

[0074] Slowly add the mixed 2-hydroxy-4-methoxybenzophenone and 3,5-di-tert-butyl-4-hydroxyphenylpropionate into the dispersed titanium dioxide nanoparticle solution while stirring;

[0075] 0.75 kg of butylated hydroxytoluene was added to the 2-hydroxy-4-methoxybenzophenone, 3,5-di-tert-butyl-4-hydroxyphenylpropionate and titanium dioxide nanoparticle solution, and stirring was continued to ensure that the components were evenly mixed;

[0076] The above solution is transferred to a rotary evaporator to evaporate excess solvent until dry ultraviolet light absorber solid powder is obtained, and then the ultraviolet light absorber solid powder is ground to obtain ultraviolet light absorber powder.

[0077] Experimental data: In order to verify the performance of the ultraviolet light absorber described in the present invention, the following comparative experiment was designed to compare the ultraviolet light absorber of the present invention with the ultraviolet light absorber currently available on the market.

[0078] Experimental conditions:

[0079] Sample 1: the ultraviolet light absorber disclosed in the present invention;

[0080] Sample 2: UV absorber UV-326;

[0081] Sample 3: UV absorber UV-327;

[0082] Solvent: ethanol;

[0083] Spectroscopic instrument: UV-Vis spectrophotometer;

[0084] Weathering test instrument: Xenon lamp aging test box.

[0085] Table 1 is the ultraviolet spectrum absorption test results of the ultraviolet light absorbers obtained in Examples 1-3:

[0086] A 0.1 wt% sample solution was prepared, and a UV-Vis spectrophotometer was used to perform an ultraviolet spectrum test in the range of 200-400 nm, and the absorption peak and absorption intensity were recorded.

[0087]

[0088] Table 2 shows the weather resistance test results of the UV absorbers obtained in Examples 1-3:

[0089] The sample was coated on the surface of the polymer film and placed in a xenon lamp aging test box to simulate the outdoor environment for an aging test. The test time was 100 hours and the absorbance changes of the sample were recorded.

[0090]

[0091] It can be seen from Table 1 and Table 2 that the absorption intensity of the three embodiments of Sample 1 in the 200-400nm band is significantly higher than that of Sample 2 and Sample 3, indicating that the ultraviolet light absorber of the present invention has a wider absorption band and higher absorption efficiency; in the weather resistance test, the absorbance of the three embodiments of Sample 1 changes slightly, and even after 100 hours of aging test, the absorbance only decreases by 0.25. The absorbance of Sample 2 and Sample 3 decreases significantly, indicating that Sample 1 has better weather resistance.

[0092] In summary, the ultraviolet light absorber and the preparation method thereof provided by the present invention have the following technical effects:

[0093] 1. The ultraviolet light absorber of the present invention has a wide absorption band, high absorption efficiency and good weather resistance;

[0094] 2. The ultraviolet light absorber of the present invention has good ultraviolet light absorption performance in the range of 200-400nm.

[0095] The technical means disclosed in the scheme of the present invention are not limited to the technical means disclosed in the above-mentioned implementation mode, but also include technical schemes composed of any combination of the above-mentioned technical features. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications are also regarded as the protection scope of the present invention.

Claims

1. A UV absorber, characterized in that: In parts by weight, it includes the following components: Sunscreen: 20-30 parts; Ester antioxidant: 10-20 parts; Titanium dioxide nanoparticles: 5-15 parts; Antioxidant: 0.5-1 part; Solvent: 50-60 parts.

2. The ultraviolet light absorber according to claim 1, characterized in that: The sunscreen is 2-hydroxy-4-methoxybenzophenone.

3. The ultraviolet light absorber according to claim 2, characterized in that: The antioxidant is butylated hydroxytoluene.

4. The ultraviolet light absorber according to claim 3, characterized in that: The solvent includes one or more of ethanol and ethyl acetate.

5. The ultraviolet light absorber according to claim 4, characterized in that: The ester antioxidant is 3,5-di-tert-butyl-4-hydroxyphenylpropionate.

6. A method for preparing an ultraviolet light absorber according to any one of claims 1 to 5, characterized in that: The steps include: S1. Preparation of precursor material: 20-30 parts of 2-hydroxy-4-methoxybenzophenone are placed in a reaction container; and 10-20 parts of an ester antioxidant are added to the reaction container and mixed thoroughly; S2. Dispersion of nanoparticles: Dispersing 5-15 parts of titanium dioxide nanoparticles in 50-60 parts of solvent to ensure that the nanoparticles are fully and evenly dispersed in the solvent; S3, initial mixing reaction: slowly adding the precursor material mixed in step S1 to the titanium dioxide nanoparticle solution dispersed in step S2, while keeping stirring; S4, secondary mixing reaction: gradually add 0.5-1 part of antioxidant to the mixture in step S3, and continue stirring to ensure that all components are evenly mixed; S5, solvent evaporation: transferring the solution in step S4 to an evaporation device to evaporate excess solvent until a dry UV absorber solid powder is obtained; S6. Powder grinding: grinding the obtained UV absorber solid powder to obtain UV absorber powder.

7. The method for preparing an ultraviolet light absorber according to claim 6, characterized in that: In the step S2, an ultrasonic disperser is used for ultrasonic dispersion for 30-60 minutes.

8. The method for preparing an ultraviolet light absorber according to claim 7, characterized in that: The stirring speed in the step S3 is 300-500 rpm, and the stirring time in the step S4 is 30-60 min.

9. The method for preparing an ultraviolet light absorber according to claim 8, characterized in that: The evaporation device in step S5 is a rotary evaporator, and rotary evaporation is performed at 50°C-70°C.

10. The method for preparing an ultraviolet light absorber according to claim 9, characterized in that: The grinding in step S6 is performed using a ball mill and the grinding is performed for 2-4 hours.

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