New method for preparing solid lignin quaternary ammonium salt and application of solid lignin quaternary ammonium salt
A quaternary ammonium salt and lignin technology, applied in the field of lignin, can solve the problems of large amount of solvent used, many reaction steps, and reduced water solubility, etc., and achieve the effect of short reaction route, mild reaction conditions, and easy control
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[0049] Example 1
[0050] 1) Weigh 4.6 g of 33% trimethylamine aqueous solution into a single-necked flask, stir for 15 minutes in an ice-salt bath at -5°C, then weigh 2.0 g of epichlorohydrin and gradually add it dropwise to the trimethylamine aqueous solution . After the addition is complete, stirring is continued for 30 minutes, and then placed in a water bath at 40° C., and stirred and reacted for 2 hours to obtain a pale yellow epoxypropyl quaternary ammonium salt intermediate. The molar ratio of trimethylamine and epichlorohydrin is 1.24:1.
[0051] 2) Weigh 2.5g of alkali lignin into a three-necked flask, add 8mL of distilled water, add 0.05g of ammonium persulfate after heating to 50°C, stir for a while, add the prepared epoxypropyl quaternary ammonium salt intermediate, and stir to react After 3.5h, a black lignin quaternary ammonium salt solution was obtained. The molar ratio of the quaternary ammonium salt intermediate to the alkali lignin is 1.45:1, and the amount of...
Example Embodiment
[0060] Example 2
[0061] Weigh 0.7g of triethylamine liquid into a single-necked flask, stir for 10min in an ice-salt bath at 0°C, then weigh 1.0g of epichlorohydrin and gradually add it dropwise to triethylamine. After the addition is completed, stirring is continued for 30 minutes, and then placed at room temperature, and stirred and reacted for 3 hours to obtain a pale yellow epoxypropyl quaternary ammonium salt intermediate. The molar ratio of triethylamine and epichlorohydrin is 1.11:1.
[0062] Weigh 1.2g alkali lignin into a three-necked flask, add 5mL distilled water, add 0.02g potassium persulfate after heating to 60℃, stir for a while, add the prepared epoxypropyl quaternary ammonium salt intermediate, stir and react for 3h , Get black lignin quaternary ammonium salt solution. The molar ratio of the quaternary ammonium salt intermediate to the alkali lignin is 1.74:1, and the catalyst dosage is 1.6% of the alkali lignin mass.
[0063] The prepared lignin quaternary ammo...
Example Embodiment
[0065] Example 3
[0066] Weigh 8.1 g of 33% trimethylamine aqueous solution into a single-necked flask, stir for 15 min in an ice-salt bath at -10°C, then weigh 3.0 g of epichlorohydrin and gradually add it dropwise to the trimethylamine aqueous solution. After the addition is complete, stirring is continued for 30 minutes, and then placed in a 35° C. water bath, and stirred for 3 hours to obtain a pale yellow epoxypropyl quaternary ammonium salt intermediate. The molar ratio of triethylamine and epichlorohydrin is 1.41:1.
[0067] Weigh 3.0g of alkali lignin into a three-necked flask, add 10mL of distilled water, add 0.15g of cerium ammonium nitrate after heating to 70°C, stir for a while, add the prepared epoxypropyl quaternary ammonium salt intermediate, stir and react for 4h , To obtain black lignin quaternary ammonium salt solution. The molar ratio of the quaternary ammonium salt intermediate and alkali lignin is 1.81:1, and the amount of catalyst is 5% of the mass of alkal...
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