Method of increasing alkaline lignin sulfonation yield
A technology of alkali lignin and sulfonation, applied in the field of improving the reaction activity of alkali lignin, can solve the problems of not being green and environmental protection, water pollution treatment pressure increases, etc., to achieve improved sulfonation efficiency, increased reaction activity, and easy recycling Effect
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Embodiment 1
[0022] Get the alkali lignin (purity is 85%, particle diameter is 80 meshes, water content is 3%) extracted from wheat straw caustic soda anthraquinone pulping black liquor, add 1-ethyl-3-methylimidazole acetate and mix pre- After the treatment, deionized water is added to stop the reaction, followed by centrifugation (3000r / min) and freeze-drying to obtain the pretreated alkali lignin. Perform vacuum distillation to recover 1-ethyl-3-methylimidazolium acetate. The treatment conditions are as follows: the amount of 1-ethyl-3-methylimidazole acetate is 400% of the mass of dry alkali lignin, the treatment temperature is 80° C., and the treatment time is 60 minutes. The sulfonation modification process of lignin is as follows: the alkali lignin sample after pretreatment is added into deionized water, the consumption of water is 300% of lignin quality, magnetic stirring (300r / min, 20min), heating to 95 ℃, Add hydrogen peroxide, control the temperature at 95°C, react for 1 hour, t...
Embodiment 2
[0028] Get the alkali lignin (purity is 80%, particle diameter is 85 orders, water content is 1%) that eucalyptus wood alkaline sulfurous acid pulping black liquor extracts, add 1-ethyl-3-methylimidazole acetate Mixing pretreatment, adding deionized water after the treatment is completed to terminate the reaction, followed by centrifugation (rotating speed 3200r / min), freeze-drying to obtain the pretreated alkali lignin. Perform vacuum distillation to recover 1-ethyl-3-methylimidazolium acetate. The treatment conditions are as follows: the amount of 1-ethyl-3-methylimidazole acetate is 450% of the mass of dry alkali lignin, the treatment temperature is 85° C., and the treatment time is 90 minutes. The sulfonation modification process of lignin is as follows: the alkali lignin sample after pretreatment is added into deionized water, the consumption of water is 300% of lignin quality, magnetic stirring (300r / min, 20min), heating to 95 ℃, Add hydrogen peroxide, control the tempe...
Embodiment 3
[0034] Take commercial alkali lignin (purity is 95%, particle size is 90 mesh, water content is 2%), add 1-ethyl-3-methylimidazole acetate to mix pretreatment, add deionized water after the treatment is completed The reaction was terminated, followed by centrifugation (3500 r / min) and freeze-drying to obtain pretreated alkali lignin. Perform vacuum distillation to recover 1-ethyl-3-methylimidazolium acetate. The treatment conditions are as follows: the amount of 1-ethyl-3-methylimidazole acetate is 500% of the mass of dry alkali lignin, the treatment temperature is 90° C., and the treatment time is 120 minutes. The sulfonation modification process of lignin is as follows: the alkali lignin sample after pretreatment is added into deionized water, the consumption of water is 300% of lignin quality, magnetic stirring (300r / min, 20min), heating to 95 ℃, Add hydrogen peroxide, control the temperature at 95°C, react for 1 hour, then add formaldehyde and sodium sulfite, keep the rea...
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