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CN-121991254-A - Synergistic preparation method and application of carboxylated cellulose nanocrystalline and regenerated cellulose

CN121991254ACN 121991254 ACN121991254 ACN 121991254ACN-121991254-A

Abstract

The invention discloses a synergistic preparation method and application of carboxylated cellulose nanocrystalline and regenerated cellulose, and belongs to the technical field of cellulose nanomaterial preparation. The preparation method of the carboxylated cellulose nanocrystalline and regenerated cellulose comprises the following steps of immersing a cellulose raw material in a Lewis acid solution, then carrying out solid-liquid separation and collecting solid components to obtain cellulose pulp, dispersing the cellulose pulp in a polycarboxylic acid solution for reaction, then carrying out filtration and collecting a solid product, and treating the solid product by a method I or a method II, wherein the method I comprises the following steps of separating the solid product to obtain carboxylated cellulose nanocrystalline and regenerated cellulose, and the method II comprises the following steps of washing the solid product and carrying out suction filtration to obtain the full-cellulose composite membrane.

Inventors

  • LIU HONGXIA
  • QIN LIYUE
  • HE RUOAO
  • ZHOU CHANGBING

Assignees

  • 桂林理工大学
  • 桂林市赛路纳科技有限公司

Dates

Publication Date
20260508
Application Date
20260127

Claims (9)

  1. 1. The synergistic preparation method of the carboxylated cellulose nanocrystalline and the regenerated cellulose is characterized by comprising the following steps: (1) Soaking a cellulose raw material in a Lewis acid solution, and then carrying out solid-liquid separation to collect solid components to obtain cellulose slurry; (2) Dispersing the cellulose pulp in a polycarboxylic acid solution, reacting, and then filtering to collect a solid product; The first method comprises the following steps of separating the solid product to obtain carboxylated cellulose nanocrystalline and regenerated cellulose; The second method comprises the steps of washing the solid product, and then carrying out suction filtration to obtain the full-cellulose composite membrane.
  2. 2. The synergistic process of claim 1, wherein the cellulosic feedstock has a solids content in the lewis acid solution of from 1 to 15wt%.
  3. 3. The synergistic process as claimed in claim 1, wherein the cellulosic raw material is one or more of microcrystalline cellulose, bacterial cellulose, purified cotton, absorbent cotton, dry bleached bagasse and dry bleached wood pulp.
  4. 4. The collaborative preparation method according to claim 1, wherein the temperature of the impregnation treatment is 20-80 ℃ for 30-240min.
  5. 5. The synergistic process as claimed in claim 1, wherein the active ingredient in the lewis acid solution is one or more of aluminum trichloride, ferric trichloride, cupric dichloride, chromium chloride, zinc chloride and lithium bromide, the active ingredient in the lewis acid solution being 30 to 90% by weight.
  6. 6. The synergistic process as claimed in claim 1, wherein the cellulose pulp has a solids content in the polycarboxylic acid solution of from 1 to 15% by weight.
  7. 7. The collaborative preparation method according to claim 1, wherein the carboxylic acid concentration in the polycarboxylic acid solution is 40-80wt%, and the carboxylic acid in the polycarboxylic acid solution is at least two of citric acid, oxalic acid, succinic acid, maleic acid, fumaric acid, itaconic acid, citraconic acid, mesaconic acid and aconitic acid.
  8. 8. The collaborative preparation method according to claim 1, wherein the reaction temperature is 20-60 ℃ and the reaction time is 2-10h.
  9. 9. The collaborative preparation method according to claim 1, wherein the separation treatment comprises the steps of centrifuging the solid product, collecting supernatant to obtain carboxylated cellulose nanocrystals, and collecting the solid remaining after the centrifugation to obtain regenerated cellulose.

Description

Synergistic preparation method and application of carboxylated cellulose nanocrystalline and regenerated cellulose Technical Field The invention relates to the technical field of cellulose nano material preparation, in particular to a synergistic preparation method and application of carboxylated cellulose nanocrystalline and regenerated cellulose. Background Cellulose Nanocrystals (CNC) are widely focused on the basis of excellent mechanical properties, high specific surface area, biodegradability and reproducibility, and have important application potential in the fields of polymer composite materials, biomedical scaffolds, intelligent hydrogels and the like. However, to expand its range of applications, it is often necessary to chemically modify the CNC surface to introduce specific reactive functional groups. At present, although a TEMPO oxidation method or a persulfate oxidation method and the like can be used for preparing CNC with carboxyl, the conventional preparation method generally has the problems of insufficient environmental friendliness (such as use of toxic reagents, low atom economy and high waste discharge) of the process flow, high comprehensive production cost (such as expensive reagents, high energy consumption, limited yield and difficult continuous production), and the like, so that the large-scale and commercial application process of carboxylated cellulose nanocrystals is severely restricted. On the other hand, although regenerated cellulose materials have the performance advantages of good processability, biocompatibility and the like, the traditional preparation process is seriously dependent on a volatile, toxic or high-cost solvent system, such as carbon disulfide used in a viscose method, so that the problem of environmental pollution is easily caused, the sustainable development of the regenerated cellulose materials is limited, and the regenerated cellulose materials still need to be further improved. Therefore, the preparation process capable of simultaneously preparing the cellulose nanocrystalline and the regenerated cellulose is designed, and the bottleneck problem that the green property and the economy are difficult to be compatible in the existing process is solved. Disclosure of Invention The invention aims to provide a synergistic preparation method and application of carboxylated cellulose nanocrystalline and regenerated cellulose, so as to solve the problems in the background art. The carboxylated cellulose nanocrystal prepared by the invention not only has high-content carboxyl groups and a regular nano structure, but also has excellent self-assembly performance, and the aqueous dispersion of the carboxylated cellulose nanocrystal can be dried under the condition of low concentration to form an ordered film with iridescence effect, and the obtained regenerated cellulose has a micrometer scale. In order to achieve the above purpose, the present invention provides the following technical solutions: According to one of the technical schemes, the invention provides a synergistic preparation method of carboxylated Cellulose Nanocrystalline (CNC) and Regenerated Cellulose (RC), which comprises the following steps: (1) Soaking a cellulose raw material in a Lewis acid solution, and then carrying out solid-liquid separation to collect solid components to obtain cellulose slurry; (2) Dispersing the cellulose pulp in a polycarboxylic acid solution, reacting, and then filtering to collect a solid product; The first method comprises the following steps of separating the solid product to obtain carboxylated cellulose nanocrystalline and regenerated cellulose; The second method comprises the steps of washing the solid product, and then carrying out suction filtration to obtain the full-cellulose composite membrane. Preferably, the cellulosic feedstock has a solids content in the lewis acid solution of 1 to 15wt%. Preferably, the cellulosic raw material is one or more of microcrystalline cellulose, bacterial cellulose, purified cotton, absorbent cotton, dry bleached bagasse, and dry bleached wood pulp. Preferably, the temperature of the impregnation treatment is 20-80 ℃ and the time is 30-240min. Preferably, the active ingredient in the Lewis acid solution is one or more of aluminum trichloride (AlCl 3), ferric trichloride (FeCl 3), cupric dichloride (CuCl 2), chromium chloride (CrCl 3), zinc chloride (ZnCl 2) and lithium bromide (LiBr), and the active ingredient in the Lewis acid solution accounts for 30-90wt%. Preferably, the cellulose pulp has a solids content in the polycarboxylic acid solution of 1 to 15wt%. Preferably, the carboxylic acid concentration in the polycarboxylic acid solution is 40-80wt%, and the carboxylic acid in the polycarboxylic acid solution is at least two of citric acid, oxalic acid, succinic acid, maleic acid, fumaric acid, itaconic acid, citraconic acid, mesaconic acid and aconitic acid. Preferably, the temperature of the reaction is 20-60 ℃ and the re