Synthesis method of high-carboxylation-degree oxidized cellulose
A technology for oxidizing cellulose and a synthesis method, which is applied in the field of synthesizing oxidized cellulose, can solve problems such as limiting the application range of oxidized cellulose, achieve high carboxylation degree, improve hydrolysis efficiency, and promote the effect of oxidation process
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Embodiment 1
[0021] Step 1: Pretreatment of cellulose material: Weigh 20g of refined cotton for crushing treatment, then put the crushed refined cotton and 60g of dry ice into a ball mill jar, seal the device and perform ball milling at 400rmp speed for 3 days ; Open the sealed cover after ball milling, expose the sample to the air and emit bright light, and obtain the pretreated cellulose material;
[0022] Step 2: Multi-step oxidation process of cellulosic material: Take 10 g of pretreated cellulosic material into a container, add 10 g of NaNO 3 , put the beaker in an ice bath, and slowly add 150 mL of 15% H 2 SO 4 , stirred for 1h to obtain mixture 1; slowly add 10gKClO to mixture 1 4 , the reaction temperature was set at 30°C, the oxidation reaction time was 30min, and mixture 2 was obtained; then 15g KClO was added to mixture 2, and then 400mL of deionized water was added, the reaction temperature was set at 50°C, and the reaction time of stirring was 50min, and mixture 3 was obtain...
Embodiment 2
[0025] Step 1: Pretreatment of cellulose material: Weigh 20g of refined cotton for crushing treatment, then put the crushed refined cotton and 80g of dry ice into a ball mill jar, seal the device and perform ball milling at a speed of 600rmp for 2 days ; Open the sealed cover after ball milling, expose the sample to the air and emit bright light, and obtain the pretreated cellulose material;
[0026] Step 2: Multi-step oxidation process of cellulosic material: Take 10g of pretreated cellulosic material into a container, add 12g NaNO 3 , put the beaker in an ice bath, and slowly add 200 mL of 20% H 2 SO 4 , stirred for 1.5h to obtain mixture one; slowly add 15gKClO to mixture one 4 , the reaction temperature is set to 35°C, the oxidation reaction time is 40min, and the mixture 2 is obtained; then 20g KClO is added to the beaker of the mixture 2, and then 500mL deionized water is added, the reaction temperature is set to 55°C, and the stirring reaction time is 55min, and the m...
Embodiment 3
[0029] Step 1: Pretreatment of cellulose material: Weigh 20g of refined cotton for crushing, then put the crushed refined cotton and 90g of dry ice into a ball mill jar, seal the device and rotate it at 800rmp for 2 days ; After ball milling, open the sealed cover, expose the sample to the air and emit bright light, and obtain the pretreated sample;
[0030] Step 2: Multi-step oxidation process of cellulosic material: Take 10 g of pretreated cellulosic material into a container, add 15 g of NaNO 3 , put the beaker in an ice bath, and slowly add 250 mL of 25% H 2 SO 4 , stirred for 2h to obtain mixture one; slowly add 25gKClO to mixture one 4, the reaction temperature was set at 35°C, the oxidation reaction time was 50min, and mixture 2 was obtained; then 30g KClO was added to mixture 2, and then 700mL of deionized water was added, the reaction temperature was set at 55°C, and the stirring reaction time was 60min, and mixture 3 was obtained ;
[0031] Step 3: Subsequent pro...
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