A kind of epoxy dimer fatty acid methyl ester and its preparation method and application
A technology of epoxy dimerized fatty acid methyl ester and dimerized fatty acid methyl ester, which is applied in the direction of organic chemistry, can solve the problems of small molecular weight, poor compatibility, and single performance of plasticizers, and achieve stable product quality and plasticizing efficiency High, good thermal stability
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[0023] A preparation method of epoxy dimerized fatty acid methyl ester, the steps are:
[0024] Step 1, blend fatty acid methyl ester with catalyst (accounting for 4-10% of the mass of fatty acid methyl ester) and heat to 160-230°C, react for 3-8 hours, the reaction mixture is washed with water and fractionated by vacuum distillation to obtain an intermediate product Dimerized fatty acid methyl ester; step 2, according to dimerized fatty acid methyl ester: peroxygen source carrier: peroxygen source: epoxidation catalyst (n / n / n / w) is 1:(0.5~0.8):(1~ 2): (0.01~0.04) proportional sampling. Mix and stir dimer fatty acid methyl ester, peroxyl group carrier and epoxidation catalyst and heat up to 50-70°C, then add the peroxygen source dropwise at a rate of 15-30ml / h, continue the heat preservation reaction for 2-4h, separate and The epoxidation catalyst is recovered to obtain the crude product of epoxy dimer acid methyl ester, and then the finished product of epoxy dimer acid methy...
Embodiment 1
[0035] Step 1: Add 50g of fatty acid methyl ester and 2g of anhydrous aluminum chloride into a 250mL four-necked flask respectively, pass in nitrogen gas to reduce the occurrence of side reactions in the reaction system, stir and heat to 180°C, react for 5h, and use 50°C for the reaction mixture ℃ mass concentration is 2% sodium carbonate solution washing and filtering to remove the catalyst, and carry out vacuum distillation at 190 ℃, 0.08MPa condition, obtain intermediate product dimerized fatty acid methyl ester;
[0036] Step 2: Weigh 20g of dimerized fatty acid methyl ester, 0.9g of formic acid and 0.4g of p-toluenesulfonic acid, add them into a three-necked flask equipped with a condenser, a stirring rod and a thermometer, stir and raise the temperature to 50°C at a speed of 15ml / h Add 4.3g of hydrogen peroxide (50%) dropwise. After the dropwise addition, the reaction temperature is raised to 65° C. to continue the reaction for 4 h; after the reaction, the crude product i...
Embodiment 2
[0038] Step 1: Add 50g of fatty acid methyl ester and 3g of anhydrous aluminum chloride into a 250mL four-necked flask respectively, pass in nitrogen gas to reduce the occurrence of side reactions in the reaction system, stir and heat to 210°C, react for 4h, and use the reaction mixture for 70 ℃ mass concentration is 2% sodium carbonate solution washing and filtering to remove the catalyst, and carry out vacuum distillation at 190 ℃, 0.08MPa condition, obtain intermediate product dimerized fatty acid methyl ester;
[0039]Step 2: Weigh 20g of dimerized fatty acid methyl ester, 0.95g of formic acid and 0.5g of p-toluenesulfonic acid, add them into a three-necked flask equipped with a condenser tube, a stirring rod and a thermometer, stir and heat up to 50°C, at a speed of 20ml / h Add 4.3g of hydrogen peroxide (50%) dropwise. After the dropwise addition, the reaction temperature is raised to 65° C. to continue the reaction for 3 h; after the reaction, the crude product is left to ...
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