AOE intermediate, hydroxy acrylic resin containing AOE intermediate and preparation method of hydroxy acrylic resin
A technology of hydroxyacrylic acid and methacrylic acid, applied in the field of coatings, can solve the problems of not meeting environmental protection requirements, high solvent content, low solid content, etc., and achieves the effect of protecting light stability, strong anti-ultraviolet ability, and satisfying environmental protection
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Embodiment 1
[0050] Take glycidyl tert-carbonate 530kg, organotin catalyst stannous octoate 350g, antioxidant tris(2,4-di-isobutylphenol) phosphite 3kg and triphenyl phosphite 700g, join in the reactor, Introduce nitrogen protection and heat up. When the temperature rises to 90°C, add 160kg of methacrylic acid and 70g of hydroquinone dropwise, and control the dropping temperature between 80°C and 100°C in 25 to 40 minutes, then keep the temperature at 90°C to 100°C for 2 hours After the determination of the acid value ≤ 15mgKOH / g, the temperature is lowered, and the nitrogen gas is sealed for standby to prepare the AOE intermediate. The schematic diagram of the chemical reaction for the preparation of AOE intermediates is shown in figure 1 shown.
[0051] 2. Preparation of hydroxyacrylic resin
Embodiment 2
[0053] A preparation method of hydroxyacrylic resin, comprising the following steps:
[0054]S11, AOE intermediate 155kg, β-hydroxypropyl acrylate (HPA) 95kg, tert-butyl methacrylate (TBMA) 80kg, n-butyl acrylate (BMA) 60kg, methyl methacrylate (MMA) 90kg, styrene (St) 170kg of each monomer is metered into the batching tank and mixed uniformly to form a mixture. 1 / 10 of the mixture is put into the reactor, and then 50kg of xylene, 5kg of benzophenone ultraviolet light absorber, and dimethacrylic acid are added. 7 kg of ethylene glycol ester (EGDMA-DMM) and 1.4 kg of 1 / 5 di-tert-amyl peroxide (BTA) were stirred and heated up under nitrogen protection.
[0055] S12. Control the temperature rise at 130-140°C and add 5.6 kg of the remaining 9 / 10 mixture and the remaining 4 / 5 of di-tert-amyl peroxide (BTA) and stir evenly. The adding time is controlled at 4.5-5.0 hours. Add the dodecyl mercaptan chain transfer agent and butyl acetate dropwise at the same time to adjust the reactio...
Embodiment 3 and 4
[0059] In Examples 3 and 4, the proportioning ratio of the hydroxyacrylic resin is shown in Table 1, and the preparation method is the same as in Example 2.
[0060] The composition and proportioning of table 1 embodiment 2-4 and commercially available resin
[0061] Raw material / Example (kg) Example 2 Example 3 Example 4 Market Resin 1 Market Resin 2 acrylic acid - - - 20 8 Glycidyl tertiary carbonate - - - 50 - AOE intermediate 156 156 156 - - β-hydroxypropyl acrylate 95 95 95 150 140 Benzophenone (ultraviolet light absorber) 6 - - - 0 Benzotriazole (ultraviolet light absorber) - 5 5 - 0 tert-butyl methacrylate 80 - 40 - 0 Methyl methacrylate 90 90 90 200 120 Butyl acrylate - - - - 40 cyclohexyl methacrylate - 80 40 - - n-Butyl methacrylate 60 60 60 150 130 Ethylene glycol dimethacrylate 7 7 7 - 0 Styrene) 170 170 170 110 160 ...
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