Process method for preparing epoxy fatty acid ester based on double liquid phase extraction technology
A technology of epoxy fatty acid ester and extraction technology, which is applied in the field of epoxy plasticizer epoxy fatty acid methyl ester, can solve the problems of discontinuous industrial process and difficult product separation, and achieves reduction of reaction mass transfer resistance and epoxy conversion. High rate, less corrosive effect
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Embodiment 1
[0037] Example 1 : figure 1 For the process flow diagram of preparing epoxy fatty acid ester based on two-liquid phase extraction technology, the specific steps are as follows:
[0038] Step 1 Add 50g of cottonseed powder into a three-necked flask, mix with 225ml of methanol containing 0.1% citric acid and 125ml of petroleum ether, stir at 30°C for 45 minutes, separate the solid from the liquid, and transfer the mixed solution to a separatory funnel for static Set the layers, the methanol phase in the lower layer is recovered by distillation, and the liquid in the upper layer is the petroleum ether phase containing cottonseed oil.
[0039] Step 2 Mix the petroleum ether phase containing cottonseed oil prepared in step 1 with 0.3 g of potassium hydroxide and 10 ml of methanol into the reaction kettle, stir and heat to 60° C. for 2 hours to react. After the reaction is over, let stand to separate layers. The upper layer is fatty acid methyl ester, and the lower layer is glyc...
Embodiment 2
[0041] Example 2 : Step 1: Add 50g of cottonseed powder into a three-necked flask, mix with 250ml of methanol containing 0.1% citric acid and 150ml of n-hexane, stir at 30°C for 45 minutes, separate the solid from the liquid, and move the mixture to a separatory funnel After standing for stratification, the methanol phase in the lower layer is recovered by distillation, and the liquid in the upper layer is the n-hexane phase containing cottonseed oil.
[0042] Step 2 is the same as step 2 of embodiment 1.
[0043]Step 3 is with the fatty acid methyl ester that makes in the step 2 and 5g formic acid and 1.2g acidic ion exchange resin
[0044] Add it into the reaction kettle, slowly add 28g of hydrogen peroxide dropwise, react at 60°C for 3.5h, let it stand for stratification, take the upper layer solution and wash it with water until it is neutral, and recover n-hexane by distillation under reduced pressure to obtain the target product epoxy fatty acid methyl ester . After ...
Embodiment 3
[0045] Example 3 : Step 1: Add 50g of cottonseed powder into a three-necked flask, mix with 300ml of methanol containing 0.1% citric acid and 150ml of isohexane, stir at 40°C for 40 minutes, separate the solid from the liquid, and move the mixture to a separatory funnel After standing for stratification, the methanol phase in the lower layer is recovered by distillation, and the liquid in the upper layer is the isohexane phase containing cottonseed oil.
[0046] Step 2 is the same as step 2 of embodiment 1.
[0047] Step 3 Add the fatty acid methyl ester prepared in step 2, 4g of formic acid and 1.5g of acidic ionic liquid into the reaction kettle, slowly add 16g of hydrogen peroxide dropwise, react at 60°C for 3.5h, let stand to separate layers, and take the upper layer The solution was washed with water until neutral, and the isohexane was recovered by distillation under reduced pressure to obtain the target product epoxy fatty acid methyl ester. After testing, the epoxy ...
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Abstract
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