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CN-121976389-A - Carboxymethyl cellulose fiber loaded with active substances and preparation method thereof

CN121976389ACN 121976389 ACN121976389 ACN 121976389ACN-121976389-A

Abstract

The invention discloses a carboxymethyl cellulose fiber loaded with active substances and a preparation method thereof, wherein the cellulose fiber is taken as a raw material, fully swelled by alkalization treatment to generate cellulose sodium salt, then subjected to etherification reaction with chloroacetic acid under a controllable condition to generate carboxymethyl cellulose fiber fibrils, then introduced with the active substances, and subjected to aftertreatment in a low-temperature environment, so that the active substances are uniformly loaded on the surface and the inside of the fiber and stably combined, and the biological activity and the functional characteristics of the fiber are effectively maintained. In the low-temperature post-treatment step, deionized water is firstly used for cleaning for a plurality of times, so that the purposes of enhancing the loading and release performance of active substances are achieved. Then stirring at low temperature, which is favorable for embedding the active substance into the fiber network through the synergistic effect of hydrogen bond and carboxymethyl, and ensures that the active substance is uniformly adsorbed on the surface and pore structure of the fiber fibrils. Finally, the temperature and time during the drying process are tightly controlled to preserve the activity of the active substance.

Inventors

  • XIAO JUN

Assignees

  • 佛山合众无纺新材料有限公司

Dates

Publication Date
20260505
Application Date
20260127

Claims (8)

  1. 1. A process for the preparation of an active-loaded carboxymethylated cellulosic fibre comprising the steps of: A. Mixing deionized water and absolute ethyl alcohol to prepare a first mixed solvent, and uniformly dissolving sodium hydroxide in the deionized water to prepare a sodium hydroxide solution; dispersing cellulose fibers and the sodium hydroxide solution in the first mixed solvent in sequence, stirring and carrying out alkalization reaction to obtain cellulose sodium salt; B. Sequentially adding chloroacetic acid and absolute ethyl alcohol into the cellulose sodium salt, uniformly mixing, adding alkyl trimethyl ammonium bromide, uniformly mixing again, stirring, and carrying out etherification reaction to carry out carboxymethylated cellulose fiber fibrils; C. repeatedly cleaning the carboxymethylated cellulose fiber by deionized water until the pH value of the cleaned cleaning solution is 6.8-7.2; Mixing deionized water and absolute ethyl alcohol to obtain a second mixed solvent, uniformly dispersing an active substance in the second mixed solvent to obtain an active solution, immersing the washed carboxymethyl cellulose fiber fibrils in the active solution, and stirring for 30-60 min, wherein the temperature of the active solution is 40-50 ℃; And (3) under a vacuum condition, placing the carboxymethyl cellulose fiber fibril immersed in the active solution at a temperature of 55-65 ℃ and drying for 2.5-3.5 hours to obtain the carboxymethyl cellulose fiber loaded with the active substance.
  2. 2. The method for preparing an active substance-loaded carboxymethylated cellulose fiber according to claim 1, wherein in step C: According to the volume ratio, in the second mixed solvent, the mixing ratio of the deionized water and the absolute ethyl alcohol is 1 (1-4); In the active solution, the mass fraction of the active substance is 0.5-2%; the stirring speed of stirring is 300-500 rpm.
  3. 3. The method for preparing the carboxymethyl cellulose fiber loaded with the active substance according to claim 1, wherein in the step A, the cellulose fiber and the sodium hydroxide solution are dispersed in the first mixed solvent in turn in an inert gas atmosphere, and are stirred and subjected to an alkalization reaction to obtain cellulose sodium salt, wherein the temperature of the alkalization reaction is 35-45 ℃ and the time is 60-90 min.
  4. 4. The method for preparing an active substance-loaded carboxymethylated cellulose fiber according to claim 1, wherein in step a: according to the mass ratio, the mixing ratio of the deionized water and the absolute ethyl alcohol in the first mixed solvent is (1-2) (50-60); According to the mass percentage, the adding amount of the sodium hydroxide in the sodium hydroxide solution is 15-25% of the adding amount of the cellulose fiber; The dispersion ratio of the cellulose fibers and the first mixed solvent is (10-15) g (50-60) mL.
  5. 5. A process for the preparation of an active substance-loaded carboxymethylated cellulosic fiber according to claim 3, characterized in that in step B: the temperature of the etherification reaction is 40-60 ℃ and the time is 2-4 hours; In the etherification reaction process, the pH value of a reaction system is maintained to be 8-9 by using an HCl solution.
  6. 6. The method for preparing the carboxymethyl cellulose fiber loaded with the active substance according to claim 1, wherein in the step B, the addition amount of chloroacetic acid is 20-30% of the addition amount of the cellulose fiber, the addition amount of absolute ethyl alcohol is 10-20% of the addition amount of the cellulose fiber, and the addition amount of alkyl trimethyl ammonium bromide is 0.02-0.05% of the addition amount of the cellulose fiber according to mass percentage.
  7. 7. The method for producing an active material-supported carboxymethylated cellulosic fiber according to claim 1, wherein in step B, the alkyl trimethylammonium bromide is any one of cetyl trimethylammonium bromide, tetradecyl trimethylammonium bromide and dodecyl trimethylammonium bromide.
  8. 8. An active material-loaded carboxymethylated cellulose fiber produced by the method for producing an active material-loaded carboxymethylated cellulose fiber according to any one of claims 1 to 7, wherein the degree of substitution of the carboxymethylated cellulose fiber fibrils is 0.7 to 1.2.

Description

Carboxymethyl cellulose fiber loaded with active substances and preparation method thereof Technical Field The invention relates to the technical field of preparation of carboxymethyl cellulose fibers, in particular to a carboxymethyl cellulose fiber loaded with active substances and a preparation method thereof. Background Cellulose is used as a natural polymer material with the most abundant reserves in the nature, and is widely applied to the fields of medicine, sanitation, environmental protection, high-end textile and the like because of being renewable, biodegradable, good in biocompatibility and rich in hydroxyl functional groups. Among them, carboxymethyl cellulose (Carboxymethyl Cellulose, CMC) is a water-soluble or water-dispersible derivative obtained by etherifying and modifying cellulose to introduce carboxymethyl, has excellent hygroscopicity, film-forming property and ion-exchange ability, and has been used for functional materials such as wound dressing, drug carrier, functional textile material, etc. However, with the continuous improvement of the performance requirements of functional fiber materials in high-end application fields such as biological medicine, intelligent slow release and environmental management, the traditional carboxymethyl cellulose fiber gradually exposes a plurality of limitations in practical application. On one hand, the inherent biocompatibility is good, but after active substances (such as antibacterial agents, growth factors, enzymes or drug molecules) are loaded, high-efficiency and stable slow release behaviors are difficult to realize, and on the other hand, the surface charge density and the pore channel structure regulation and control capability are limited, so that the adsorption capacity on target molecules is low, the selectivity is poor, and the requirements of accurate delivery or high-efficiency capture are difficult to meet. In order to improve the performance, the prior art generally adopts chemical grafting, crosslinking or blending and other means to carry out secondary modification on the carboxymethyl cellulose fiber, and introduces active functional components in the preparation process. However, the method has the common problems that (1) active substances are unevenly distributed in the fiber or on the surface and are easy to form local aggregation to influence the release kinetics and the function consistency, (2) the control accuracy requirement of modification reaction conditions (such as pH, temperature and reaction time) is high, the control accuracy is slightly deviated, namely, the degradation of a cellulose main chain or the uncontrolled substitution degree of carboxymethyl is caused, so that the mechanical property is deteriorated or the structure is collapsed, (3) in the loading process, part of active substances are inactivated due to exposure to strong acid, strong alkali or high-temperature environment, so that the biological activity or the catalytic efficiency of the final product is obviously reduced, and (4) reaction byproducts (such as unreacted cross-linking agents, salts or organic solvents) are difficult to thoroughly remove, so that the purity of the product is influenced, the cytotoxicity is possibly caused, and the application of the cellulose main chain is limited in the sensitive fields such as medical treatment. Therefore, development of a preparation method of carboxymethylated cellulose fibers with simple process, mild conditions and strong controllability is needed, and uniform loading and high activity retention of active substances can be realized on the premise of ensuring the structural integrity of the fibers, so that the comprehensive requirements of high-end application scenes on the functional fiber materials in terms of safety, stability and efficiency are met. Disclosure of Invention The invention aims to provide a carboxymethyl cellulose fiber loaded with active substances and a preparation method thereof, which can realize uniform loading and high activity retention of the active substances on the premise of ensuring the structural integrity of the fiber, and have simple steps and strong operability, thereby being beneficial to overcoming the defects in the prior art. To achieve the purpose, the invention adopts the following technical scheme: A process for the preparation of an active-loaded carboxymethylated cellulosic fibre comprising the steps of: A. Mixing deionized water and absolute ethyl alcohol to prepare a first mixed solvent, and uniformly dissolving sodium hydroxide in the deionized water to prepare a sodium hydroxide solution; dispersing cellulose fibers and the sodium hydroxide solution in the first mixed solvent in sequence, stirring and carrying out alkalization reaction to obtain cellulose sodium salt; B. Sequentially adding chloroacetic acid and absolute ethyl alcohol into the cellulose sodium salt, uniformly mixing, adding alkyl trimethyl ammonium bromide, uniformly mixing again, st