A photocuring putty and a preparation method thereof

Abstract

The application belongs to the field of new materials, and discloses a photocuring putty, which comprises photocuring resin, diluent, phenolic polymerization inhibitor, anti-sedimentation agent, pigment, filler and photoinitiator; the filler is composed of organic silicon surface modified talc powder and nano alumina; the weight ratio of the photocuring resin, nano alumina and organic silicon surface modified talc powder is 100:5-10:90-105. The photocuring resin on the market is used, the stability and strength of the filler are improved by adjusting the composition of the filler, and the problems of the photocuring resin caused by too fast surface drying and curing, such as the increase of shrinkage rate and the decrease of adhesion rate, are effectively inhibited. Meanwhile, the application also discloses a preparation method of the putty.

Description

Technical Field

[0001] This invention belongs to the field of new materials, and more specifically, relates to a photocurable atomic putty and its preparation method. Background Technology

[0002] Atomic putty, also known as putty, is a relatively new product on the market. Its biggest advantages are low volatile content and high hardness after curing.

[0003] For example, patent application CN114437332A, which is entitled "Polyester Oligomers and Their Preparation Methods, Light-Cured Putty and Their Preparation Methods, Curing Methods and Applications", improves the flexibility, air-drying properties and sandability of putty by modifying the light-cured resin.

[0004] However, due to its faster curing speed, UV-cured putty requires control of excessive shrinkage and improvement of adhesion compared to traditional two-component putty. Summary of the Invention

[0005] The main objective of this invention is to provide a photocurable putty. This invention uses commercially available photocurable resin and improves the stability and strength of the filler by adjusting the composition of the filler, effectively suppressing the problems of excessively fast surface drying of the photocurable resin, increased shrinkage rate due to curing, and reduced adhesion rate.

[0006] In addition, the present invention also discloses a method for preparing atomic ash.

[0007] According to a first aspect of the present invention, a photocurable putty is provided, comprising a photocurable resin, a diluent, a phenolic polymerization inhibitor, an anti-settling agent, a pigment, a filler, and a photoinitiator; wherein the filler is composed of silicone-modified talc and nano-alumina; and the weight ratio of the photocurable resin, nano-alumina, and silicone-modified talc is 100:5-10:90-105.

[0008] In the above-mentioned photocurable putty, the diluent is styrene, and the amount of the diluent is 6-10 wt% of the amount of photocurable resin.

[0009] In the above-mentioned photocurable putty, the phenolic polymerization inhibitor is hydroquinone, and the amount of the phenolic polymerization inhibitor is 0.01 to 0.02 wt% of the amount of photocurable resin.

[0010] In the above-mentioned photocurable putty, the anti-settling agent is silica and organobentonite; the amount of silica is 0.5 to 1.5 wt% of the amount of photocurable resin; the amount of organobentonite is 0.5 to 1.5 wt% of the amount of photocurable resin.

[0011] In the above-mentioned photocurable putty, the photoinitiator is IHT-PI 4265; IHT-PI 4265 is composed of 50wt% IHT-PI TPO and 50wt% IHT-PI 1173; the photoinitiator is 1 to 3wt% of the amount of photocurable resin.

[0012] In the above-mentioned photocurable atomic putty, the talc powder is modified with a silane coupling agent;

[0013] The silane coupling agent is one or more combinations of KH550, KH560, and KH580;

[0014] The silane coupling agent is dispersed in silicone oil to form a silane coupling agent solution. The silane coupling agent solution acts on the talc powder to form a silane coupling agent coating layer on the surface of the talc powder.

[0015] Meanwhile, this invention also discloses a method for preparing photocurable atomic putty as described above, comprising the following steps:

[0016] Step 1: Add the photocurable resin to the mixing tank, along with the diluent, phenolic polymerization inhibitor, anti-settling agent, pigment, photoinitiator, and nano-alumina, and stir for 10-15 minutes;

[0017] Step 2: Add the silicone-modified talc powder to Step 1 and stir for 15-25 minutes.

[0018] In the above preparation method, the temperature of steps 1 and 2 is controlled at 40-45°C.

[0019] One of the above-described technical solutions of the present invention has at least one of the following advantages or beneficial effects:

[0020] This invention uses commercially available UV-curable resin combined with surface-modified talc to improve the compatibility between talc and UV-curable resin, thereby suppressing the shrinkage of the UV-curable resin during rapid curing and improving adhesion. At the same time, nano-alumina is used as an auxiliary filler to improve the strength of the UV-curable resin. The nano-sized alumina can fill the gaps in the talc, improving the overall strength of the putty. In addition, it can further suppress resin shrinkage and improve adhesion. Attached Figure Description

[0021] Figure 1 A photograph of the sample from Example 2;

[0022] Figure 2 A photograph of the sample in Comparative Example 1;

[0023] Figure 3 This is a photograph of the sample in Comparative Example 3. Detailed Implementation

[0024] The embodiments of the present invention are described in detail below. These embodiments are exemplary and are only used to explain the present invention, and should not be construed as limiting the present invention.

[0025] Examples and Comparative Examples

[0026] A method for preparing photocurable atomic putty

[0027] Step 1: Add the photocurable resin to the mixing tank, along with the diluent, phenolic polymerization inhibitor, anti-settling agent, pigment, photoinitiator, and nano-alumina. Stir for 10-15 minutes at a temperature of 40-45°C.

[0028] Step 2: Add the silicone-modified talc powder to Step 1 and stir for 15-25 minutes at a temperature of 40-45℃.

[0029] The modification method of talc is as follows: KH550 is added to polydimethylsiloxane to form silicone oil with a KH550 concentration of 5wt%. The silicone oil is added to talc at a weight ratio of 2:100 and stirred at high speed until the silicone oil and talc are fully mixed and homogeneous to obtain silicone-modified talc. All talc mentioned in the formula table refers to silicone-modified talc.

[0030] The UV-curable resin was purchased from AOC China / Jinling Lilians Resin Co., Ltd.

[0031] The phenolic polymerization inhibitor is hydroquinone; the diluent is styrene; the anti-settling agents are silica and organobentonite; the pigment is titanium blue violet; and the photoinitiator is IHT-PI 4265.

[0032] The relevant formulas are shown in Table 1;

[0033] Table 1 Formula Table (Unit: g)

[0034]

[0035] Comparative Example 3

[0036] The results are largely the same as in Example 2, except that the talc used in this comparative example is unmodified talc.

[0037] Comparative Example 4

[0038] Step 1: Add the light-curing resin to the mixing tank, add the diluent, phenolic polymerization inhibitor, anti-settling agent, pigment, and photoinitiator, stir for 10-15 minutes at a temperature of 40-45℃;

[0039] Step 2: Add the silicone-modified talc powder and nano-alumina to Step 1, stir for 15-25 minutes at a temperature of 40-45℃.

[0040] The formula is the same as in Example 2.

[0041] The following precautions should be taken when applying the putty of this invention:

[0042] Use solvents and polishers to thoroughly remove rust, oil, old paint film, and moisture from the surface, keeping the surface clean and dry.

[0043] The recommended curing light source for UV-cured putty is a 395nm wavelength UV-LED surface light source. The light-emitting size of the surface light source should be no less than 300mm × 250mm, the power of the surface light source should be no less than 600W, and the maximum irradiance should be no less than 600mW / cm².

[0044] As the size of the surface light source increases, the power and maximum radiation intensity requirements of the light source should be increased accordingly. The distance between the surface light source and the surface of the putty coating to be cured should not exceed 15cm to ensure sufficient irradiance on the curing surface. The farther the curing surface is from the light source, the lower the irradiance. To ensure complete curing of the putty coating, the irradiance on the surface of the putty coating during curing should not be less than 252mW / cm².

[0045] The prepared putty has a working time of no less than 2 hours under light-protected conditions. After the putty is applied, irradiate it for 3-5 minutes under a UV-LED light source, with the coating surface no more than 15 cm away from the UV-LED light source. Sanding can be done after the coating cools to room temperature.

[0046] Performance testing

[0047] The performance testing items, indicators, and qualification standards for the products of this invention are shown in Table 2 below;

[0048] Table 2 Test Items

[0049]

[0050]

[0051] All embodiments and comparative examples of the present invention passed the tests for items 01 to 08. The results for other items are shown in Table 3.

[0052] Table 3 Detection Results

[0053]

[0054] Results analysis:

[0055] 1. As can be seen from Examples 1 to 3, adding an appropriate amount of nano-alumina and surface modification of talc can improve adhesion, impact resistance and high temperature resistance.

[0056] 2. As can be seen from Comparative Examples 1 and 2, the addition of a small amount of nano-alumina can slightly improve adhesion and impact resistance, while the high-temperature resistance is significantly improved.

[0057] 3. As can be seen from Comparative Example 3, modification of talc is important for improving its compatibility with curing scenarios of photocuring. Without surface modification of talc, its adhesion, impact resistance and high temperature resistance will be significantly reduced.

[0058] 4. As can be seen from Comparative Example 4, the timing of alumina addition is also quite important.

[0059] Based on the above results, we infer that the reason for the above phenomenon is:

[0060] Nano-alumina and its addition timing, as well as the surface modification of talc, are particularly important for performance improvement. The main reason for the performance defects is that compared with traditional curing methods, the photocuring reaction has less solvent and faster curing speed. This leads to changes in the degree of cross-linking of the resin in a short period of time, resulting in more obvious shrinkage. Although this curing can improve the strength of the resin, it has a significant impact on adhesion and impact resistance. This effect is even more pronounced when the putty is in a high-temperature environment.

[0061] Nano-alumina, as a commonly used inorganic material, is widely used in coatings to improve the scratch resistance and hardness of the coating. However, it is less commonly used in putty. This invention introduces nano-alumina into the putty and pre-blends it with the resin to ensure uniform dispersion. When surface-modified talc is added, the nano-alumina partially contacts the silane coupling agent on the talc surface and further binds to the talc, preferentially filling the layered flakes of the talc. Working together with the silane coupling agent, it achieves bonding with the resin, improving bonding stability. Simultaneously, the nano-alumina in the resin strengthens the resin during curing. Therefore, the control of resin shrinkage benefits from the affinity-improving function of the silane coupling agent, the further affinity-improving function of nano-alumina, and the reinforcing effect of nano-alumina on the resin.

Claims

1. A photocurable atomic putty, characterized in that, It includes a photocurable resin, a diluent, a phenolic polymerization inhibitor, an anti-settling agent, pigments, fillers, and a photoinitiator; the filler is composed of silicone-modified talc and nano-alumina. The weight ratio of the photocurable resin, nano-alumina, and organosilicon surface-modified talc is 100:5~10:90~105; The talc powder is modified with a silane coupling agent; The silane coupling agent is one or more combinations of KH550, KH560, and KH580; The silane coupling agent is dispersed in silicone oil to form a silane coupling agent solution. The silane coupling agent solution acts on the talc powder to form a silane coupling agent coating layer on the surface of the talc powder. The preparation method of the photocurable atomic putty includes the following steps: Step 1: Add the photocurable resin to the mixing tank, along with the diluent, phenolic polymerization inhibitor, anti-settling agent, pigment, photoinitiator, and nano-alumina, and stir for 10-15 minutes; Step 2: Add the silicone-modified talc powder to Step 1 and stir for 15-25 minutes.

2. The photocurable atomic putty according to claim 1, characterized in that, The diluent is styrene, and the amount of the diluent used is 6 to 10 wt% of the amount of the light-curing resin.

3. The photocurable atomic putty according to claim 1, characterized in that, The phenolic polymerization inhibitor is hydroquinone, and the amount of the phenolic polymerization inhibitor is 0.01~0.02wt% of the amount of the photocurable resin.

4. The photocurable atomic putty according to claim 1, characterized in that, The anti-settling agent is silica and organobentonite; the amount of silica is 0.5~1.5 wt% of the amount of photocurable resin; the amount of organobentonite is 0.5~1.5 wt% of the amount of photocurable resin.

5. The photocurable atomic putty according to claim 1, characterized in that, The photoinitiator is IHT-PI 4265; the photoinitiator is 1-3 wt% of the amount of photocurable resin.

6. The photocurable atomic putty according to claim 2, characterized in that, The temperature in steps 1 and 2 is controlled at 40~45℃.

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