Catalyst prepared by utilizing paper mill black water and application of the catalyst in biodiesel preparation
A technology of biodiesel and catalyst, applied in physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, chemical/physical process, etc., can solve the problems that have not yet been reported successfully, difficult economic benefits, recovery The problem of high cost, to achieve the effect of continuous organic material source, high activity and easy separation
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Embodiment 1
[0028] Collect the black water of the paper mill, adjust the black water of the paper mill to pH 6 with 5 mol / L hydrochloric acid, then add twice the volume of 95% ethanol to precipitate lignin, and distill the filtered lignin sample at 80-100°C to Recover ethanol, then suspend with pH 2.0 hydrochloric acid solution, filter again and wash 3 times with pH 2.0 aqueous solution, and dry the sample at 55-105°C to obtain lignin. 10 g of dry lignin was pretreated with phosphoric acid solution at 60 °C for 120 min to obtain lignin with a loose structure, and the porous carbon support was carbonized at 400 °C for 5 h under the protection of an inert gas, and the porous carbon The carrier was sulfonated with 98% concentrated sulfuric acid at 150 °C for 5 h to obtain a black solid powder, which was washed with deionized water and dried to obtain a lignin-based solid acid.
[0029] XRD shows that the catalyst has an amorphous carbon structure composed of layered aromatic ring carbons, an...
Embodiment 2
[0031] Repeat Example 1 with the following differences: 10 g of recovered lignin was weighed, carbonized at 400°C for 1 h under nitrogen protection, and then sulfonated at 200°C for 2 h to obtain 5.1 g of lignin-based solid acid. Mix 14.1 g of oleic acid and 16 g of methanol in a reactor, heat to 80°C, add 0.7 g of lignin-based solid acid, stir and react at 80°C, 150 r / min for 5 h, and the esterification rate is 94.2%. The reaction solution is centrifuged to recover lignin-based solid acid, the remaining liquid phase is subjected to vacuum distillation to recover methanol, the remaining liquid phase is biodiesel, and the refined product of biodiesel is obtained through vacuum distillation. The lignin-based solid acid was washed three times with methanol and then dried.
Embodiment 3
[0033] Repeat Example 1 with the following differences: 10 g of recovered lignin was weighed, treated with phosphoric acid for 60 min, carbonized at 400°C for 1 h under nitrogen protection, and then sulfonated at 200°C for 2 h to obtain lignin Base solid acid 6.3 g. Mix 14.1 g of oleic acid and 16 g of methanol in a reactor, heat to 80 °C, add 0.7 g of lignin-based solid acid, stir and react at 80 °C, 150 r / min for 5 h, and the esterification rate is 96.5%. The reaction solution is centrifuged to recover lignin-based solid acid, the remaining liquid phase is subjected to vacuum distillation to recover methanol, the remaining liquid phase is biodiesel, and the refined product of biodiesel is obtained through vacuum distillation. The lignin-based solid acid was washed three times with methanol and then dried.
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