A kind of carboxylated cnf and preparation method thereof
A carboxylated and permanganate technology, applied in the field of carboxylated CNF and its preparation, can solve the problems of unfriendly environment, long enzymatic hydrolysis time, poor dispersibility, etc., to reduce production cost, enhance mechanical properties, and improve dispersion. sexual effect
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[0028] The preparation method of a kind of carboxylated CNF of the present invention specifically comprises the steps:
[0029] Step 1, the sulfate-bleached softwood pulp board is stirred in a hydraulic pulper for 30 minutes to disperse uniformly, and then the mass fraction of the solution is adjusted to 30% with water.
[0030] Step 2, configure 1wt% dilute sulfuric acid in a 1000mL container, add a certain amount of permanganate and pulp under stirring, the permanganate is potassium permanganate or sodium permanganate, and prepare the mass fraction of the slurry 0.8% to 1.0%, the added mass of permanganate is 0.2% to 0.5% of sulfuric acid, and the reaction is carried out at 50 to 70 DEG C for 3 to 4 hours to complete the carboxylation process of cellulose. The reaction was quenched with hydrogen peroxide to obtain a white cellulose suspension.
[0031] In step 3, the above suspension is vacuum filtered and washed with water for 3 to 5 times until the filtrate is neutral. T...
Embodiment 1
[0035] The preparation method of a kind of carboxylated CNF of the present invention specifically comprises the steps:
[0036] Step 1) The sulfate-bleached softwood pulp board is stirred in a hydraulic pulper for 30 minutes to disperse, and then the mass fraction of the pulp is adjusted to 30% with water.
[0037] Step 2) Configure 1wt% dilute sulfuric acid in a 1000mL container, add a certain amount of potassium permanganate and pulp under stirring, the mass fraction concentration of the prepared slurry is 0.8%, and the added mass of potassium permanganate is 10% of sulfuric acid. 0.2%, react at 70℃ for 3h to complete the carboxylation of cellulose. The reaction was quenched with hydrogen peroxide to obtain a white cellulose suspension.
[0038] Step 3) Filter and wash the above suspension three times until the filtrate is neutral. The upper white paste-like solid oxidation product was collected.
[0039] Step 4), taking the above product and dispersing it in deionized wa...
Embodiment 2
[0043] The preparation method of a kind of carboxylated CNF of the present invention specifically comprises the steps:
[0044] Step 1) The sulfate-bleached softwood pulp board is stirred in a hydraulic pulper for 30 minutes to disperse, and then the mass fraction of the pulp is adjusted to 30% with water.
[0045] Step 2) Configure 1wt% dilute sulfuric acid in a 1000mL container, add a certain amount of sodium permanganate and pulp under stirring, the mass fraction of the prepared slurry is 1.0%, and the amount of sodium permanganate added is 0.5% of dilute sulfuric acid. %, react at 50°C for 4h to complete the carboxylation of cellulose. The reaction was quenched with hydrogen peroxide to obtain a white cellulose suspension.
[0046] Step 3) Filter and wash the above suspension for 4 times until the filtrate is neutral. The upper white paste-like solid oxidation product was collected.
[0047] Step 4), taking the above product and dispersing it in deionized water for ultr...
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