Preparation method of CMCLi and application thereof
A technology of reaction and ionic liquid, which is applied in the field of CMCLi preparation, can solve the problems of carboxymethyl cellulose lithium with many by-products and low purity, and achieve the effect of high degree of substitution, high purity and easy biodegradation
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Embodiment 1
[0034] The preparation method of CMCLi comprises the steps,
[0035] Step 1: Dissolve 5 parts of microcrystalline cellulose with 50 parts of 1-butyl-3-methylimidazolium chloride salt BMImCl at 140°C, then add 1 part of lithium hydroxide and mix evenly to obtain the first mixed solution;
[0036] Step 2: keep the temperature at 50° C., add 1 part of chloroacetic acid to the first mixed solution for reaction, and post-process after the reaction to obtain CMCLi.
[0037] During post-treatment, the crude CMCLi was neutralized with glacial acetic acid to a pH of 6, precipitated with methanol, washed with methanol, filtered to remove liquid, dried at 60°C, and pulverized to obtain CMCLi.
Embodiment 2
[0039] The preparation method of CMCLi comprises the steps,
[0040] Step 1: Dissolve 5 parts of microcrystalline cellulose at 140°C with 80 parts of 1-methylimidazolium chloride salt MImCl, then add 2 parts of lithium hydroxide and mix evenly to obtain the first mixed solution;
[0041] Step 2: keep the temperature at 55° C., add 2 parts of chloroacetic acid to the first mixed solution for reaction, and post-process after the reaction to obtain CMCLi.
[0042] During post-treatment, the crude CMCLi is neutralized with glacial acetic acid to a pH of 6, precipitated through a mixture of methanol and water, washed with a mixture of methanol and water, filtered to remove the liquid, dried at 70°C, and pulverized to obtain CMCLi. Methanol accounts for 65% of the mass of the mixture.
Embodiment 3
[0044] The preparation method of CMCLi comprises the steps,
[0045] Step 1: Dissolve 5.1 parts of microcrystalline cellulose with 100 parts of 1-ethyl-3-methylimidazolium chloride salt EMImCl at 120°C, then add 3 parts of lithium hydroxide and mix evenly to obtain the first mixed solution;
[0046] Step 2: keep the temperature at 60° C., add 3 parts of chloroacetic acid to the first mixed solution for reaction, and post-process after the reaction to obtain CMCLi.
[0047] During the post-treatment, the crude CMCLi is neutralized with glacial acetic acid to a pH of 6, precipitated through a mixture of ethanol and water, washed with a mixture of ethanol and water, filtered to remove the liquid, dried at 75°C, and pulverized to obtain CMCLi. Wherein ethanol accounts for 70% of the mixed solution quality.
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