Terpene-based macroporous adsorption resin and preparation method thereof
A pore adsorption and terpene-based technology, which is applied in the field of macroporous adsorption resin and its preparation, can solve the problems of low extraction rate, complicated equipment, styrene and divinylbenzene residues, etc., and achieves easy availability of raw materials and low price Effect
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Embodiment 1
[0077] 1. Preparation of Terpene Maleic Anhydride
[0078] Put 100mL α-pinene, 200mL ethyl acetate solvent, 0.84g phosphomolybdic acid and 60.5g maleic anhydride in a 500mL three-neck round bottom flask, install a thermometer, reflux condenser and stirrer, and react in a water bath at 80°C for 4h. Cool to room temperature, add 50mL of cyclohexane, wash with saturated aqueous sodium chloride until neutral light yellow liquid, remove polymaleic acid and catalyst, then rectify at -0.1Mpa under reduced pressure, collect 170-180 °C fraction to obtain 46.5 g of terpene maleic anhydride.
[0079] 2. Preparation of terpene di(β-hydroxyethyl) maleate
[0080] Get 20g of terpene maleic anhydride prepared by step 1, place in a 250mL three-necked round-bottomed flask, add 1.6g of p-toluenesulfonic acid catalyst and 15mL of ethylene glycol, install a thermometer, water separator, stirrer and reflux Condensate the tube, start the agitator, heat, control the reaction temperature at 120-140...
Embodiment 2
[0089] 1. Preparation of Terpene Maleic Anhydride
[0090] Terpene maleic anhydride was prepared according to step 1 in Example 1.
[0091] 2. Preparation of terpene di(β-hydroxyethyl) maleate
[0092] Get 50g terpene maleic anhydride prepared by step 1, place in a three-necked round-bottomed flask of 500mL, add 1.5g p-toluenesulfonic acid catalyst and 47.5mL ethylene glycol, install thermometer, water separator, stirrer and Reflux the condenser, start the agitator, heat, control the reaction temperature at 120-140°C, heat the reaction for 4 hours, stop the reaction, cool to room temperature, wash the product repeatedly with deionized water, remove the catalyst and unreacted ethylene glycol, and then Evaporate and remove water with a rotary evaporator, and measure the acid value of the product to be 13.7mgKOH g -1 ;
[0093] 3. Preparation of terpene maleate bis(β-acryloyloxyethyl)ester
[0094] Get 40g of terpene maleate di(β-hydroxyethyl) prepared by step 2 in a 250mL th...
Embodiment 3
[0101] 1. Preparation of Terpene Maleic Anhydride
[0102] Terpene maleic anhydride was prepared according to step 1 in Example 1.
[0103] 2. Preparation of terpene di(β-hydroxyethyl) maleate
[0104] Get 100g of terpene maleic anhydride prepared by step 1, place in a 500mL three-necked round-bottomed flask, add 6g of p-toluenesulfonic acid catalyst and 95mL of ethylene glycol, install a thermometer, water separator, stirrer and reflux condensing tube, start the stirrer, heat, control the reaction temperature at 120-140°C, heat the reaction for 4h, stop the reaction, cool to room temperature, wash the product repeatedly with deionized water, remove the catalyst and unreacted ethylene glycol, and then use a rotary The evaporator evaporates and removes water, and the acid value of the product measured is 14.2mgKOH g -1 ;
[0105] 3. Preparation of terpene maleate bis(β-acryloyloxyethyl)ester
[0106] Get 80g of terpene maleate di(β-hydroxyethyl) prepared by step 2 in a 500m...
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