Preparation method of a biodegradable lignin-based microporous molecular sieve with high oil absorption rate
A microporous molecular sieve and biodegradable technology, which is applied in the field of preparation of biodegradable lignin-based microporous molecular sieves with high oil absorption rate, can solve the problems of low primary oil absorption rate, low three-dimensional network chemical crosslinking structure, water absorption and oil absorption performance Interference and other problems, to achieve the effect of uncomplicated treatment method, simple recycling process and wide application range
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Embodiment 1
[0033] Under the reaction temperature of 90℃, dissolve 1g of lignin in 50g of pyridine / dioxane mixture (pyridine:dioxane=1:10, mass ratio), add dropwise appropriate amount of acetic anhydride reagent (acetic anhydride and The molar ratio of the hydroxyl groups in the lignin is 1:2), and the stirring is continued to cause the hydroxyl groups in the lignin to undergo an acetylation reaction with acetic anhydride. The reaction time is 2h. The product is cooled to room temperature, filtered, washed with water three times, and dried to obtain acetyl lignin. Under the condition of reaction temperature 70℃, dissolve acetyl lignin in a mixture of pyridine / triethoxychlorosilane (pyridine:triethoxychlorosilane=1:5, mass ratio), in which triethoxychlorosilane The molar ratio with the hydroxyl group in acetyl lignin is 1:1. Continue to stir to make the hydroxyl group in the acetyl lignin react with triethoxychlorosilane. The reaction time is 12 hours. After the product is cooled to room ...
Embodiment 2
[0036] Refer to Example 1 to prepare acetyl lignin, and then dissolve the acetyl lignin in a mixture of pyridine / triethoxychlorosilane (pyridine:triethoxychlorosilane=1:10) at a reaction temperature of 70°C. The molar ratio of triethoxychlorosilane to hydroxyl groups in acetyl lignin is 1:1. Continue to stir to make the hydroxyl group in the acetyl lignin react with triethoxychlorosilane, and the reaction time is 10h. After the product is cooled to room temperature, filtered, washed with water three times, and dried to obtain silyl acetyl lignin. Add the silyl acetyl lignin to the 4A type microporous molecular sieve suspension (mass concentration 10%) dissolved in N,N-dimethylformamide (DMF) at room temperature, in which the hydroxyl and silyl acetyl lignin in the molecular sieve The molar ratio of ethoxy groups is 1:1. N 2 Under protection, the temperature is raised to 150℃ and the reaction is refluxed for 36 hours. After the product is cooled to room temperature, filtered, ...
Embodiment 3
[0039] Refer to Example 1 to prepare acetyl lignin, and then dissolve the acetyl lignin in a pyridine / triethoxychlorosilane mixed solution (pyridine:triethoxychlorosilane=1:3) at a reaction temperature of 70°C, wherein The molar ratio of triethoxychlorosilane to hydroxyl groups in acetyl lignin is 1:1. Continue to stir to make the hydroxyl group in the acetyl lignin react with triethoxychlorosilane. The reaction time is 12 hours. After the product is cooled to room temperature, filtered, washed with water three times, and dried to obtain silyl acetyl lignin. Add silyl acetyl lignin to a suspension of type 5A microporous molecular sieve (mass concentration 5%) dissolved in xylene at room temperature. The molar ratio of the hydroxyl group in the molecular sieve to the ethoxy group in the silyl acetyl lignin is 1: 1. N 2 Under protection, the temperature is raised to 140℃ and the reaction is refluxed for 24 hours. After the product is cooled to room temperature, filtered, washed...
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