A method for extracting dicyclopentadiene in ethylene cracking C9
A dicyclopentadiene and ethylene cracking technology, applied in chemical instruments and methods, purification/separation of hydrocarbons, purification/separation of chemical changes, etc., can solve problems such as high energy consumption, intensified coking and other side reactions, and large investment. Achieve low energy consumption, avoid tar and polymer, and low reaction temperature
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Embodiment 1
[0040] 10 grams of hydroquinone and 50 grams of cyclohexane were placed in a 250 ml four-necked flask equipped with a thermometer, a constant pressure dropping funnel and a reflux condenser, and 10 grams of chlorosulfonic acid was added dropwise at room temperature and under nitrogen protection. , then heated to 70 ～ Stir at 75°C for 4 hours, then cool to room temperature, add 50ml of water to dilute, and neutralize to pH=5 with saturated sodium hydroxide solution, clarify and separate phases, separate the lower aqueous phase, and place it in a 250ml flask , plus 40 grams of highly active MnO 2 , stirred at room temperature for 12 hours, filtered to remove solids, and the filtrate was distilled under reduced pressure to remove water and other low boilers to obtain 14.7 grams of sodium benzoquinone sulfonate.
Embodiment 2
[0042] Put 10 grams of hydroquinone and 50 grams of cyclohexane into a 250 ml four-necked flask equipped with a thermometer, a constant pressure dropping funnel and a reflux condenser, and add 8 ml of 98% concentrated solution dropwise at room temperature and under nitrogen protection. Sulfuric acid, then heated to 80°C and stirred for 30 minutes, then cooled to room temperature, diluted with 50 ml of water, and neutralized with saturated potassium hydroxide solution to pH = 5, clarified and separated, separated the lower aqueous phase, and placed it in a In a 250ml flask, add 50ml of 30% hydrogen peroxide 2 , stirred at room temperature for 4 hours, and distilled under reduced pressure to remove water and other low boilers to obtain 15.2 grams of potassium benzoquinone sulfonate.
Embodiment 3
[0044] Select sodium benzoquinone sulfonate and LnCl with different concentrations and ratios 3 , tetrabutylammonium chloride and water are used to carry out single-stage extraction of C9, as shown in the table below:
[0045] Table 1
[0046]
[0047] Add the extractant and C9 into the extraction device at a volume ratio of 4:1, heat to 95-100°C and stir and reflux for 4 hours. After clarification and phase separation, separate the upper oil phase C9, and measure the DCPD content in it by gas chromatography external standard method content; the separated loaded extraction water phase is placed in the extraction agent regeneration device, and rectified at 95-100 ° C for 4 hours, and the distillate is layered to remove water and dried to obtain DCPD, while the water phase contains regenerated water-soluble benzoquinone sulfonic acid Sodium and other extractant components can be recycled, and the DCPD concentration in C9 before and after extraction is shown in the table abov...
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