A cellulose solution and its preparation method

A cellulose solution and cellulose technology, applied in the field of cellulose, can solve the problems of restricting the high-value utilization of cellulose, increasing the difficulty of cellulose processing, and difficult to dissolve cellulose, etc., to avoid cellulose degradation, promote dissolution, inhibit The effect of cellulose degradation

Active Publication Date: 2021-05-11
NANJING FORESTRY UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

In the process of cellulose application, the dissolution of cellulose is a technical problem, mainly because the cross-linked hydrogen bond network of cellulose molecules is extremely difficult to be destroyed, and it is difficult for conventional solvents to dissolve cellulose, which increases the difficulty of cellulose processing and is very difficult. High-value utilization of cellulose is largely limited

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  • A cellulose solution and its preparation method
  • A cellulose solution and its preparation method
  • A cellulose solution and its preparation method

Examples

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preparation example Construction

[0026] The invention provides a kind of preparation method of cellulose solution, comprises the steps:

[0027] (1) Under the condition of 15-30°C, soak the cellulose raw material in water, and then dry to obtain swollen cellulose;

[0028] (2) mixing the cellulose obtained in the step (1) with a polar organic solvent to obtain a cellulose dispersion;

[0029] (3) The cellulose dispersion obtained in the step (2) is mixed with a tetraalkyl quaternary ammonium base at 15~30° C.

[0030] Mixing under conditions to obtain a cellulose solution, the mixing is carried out under stirring, the stirring speed is 200-400r / min, and the stirring time is 2-6h.

[0031] In the present invention, unless otherwise specified, the reagents for preparing the cellulose solution are commercially available products well known to those skilled in the art.

[0032] The invention soaks the cellulose raw material in water under the condition of 15-30 DEG C, and then dries to obtain the swollen cellul...

Embodiment 1

[0047] TBAH pretreatment: Weigh 20 g of commercially available TBAH products, and treat in a rotary evaporator with a vacuum degree of -0.098 kPa at 60° C. for 60 min to remove moisture to obtain anhydrous TBAH. The DMSO was treated by vacuum distillation to obtain dehydrated DMSO.

[0048] Weigh 5.0 g of broad-leaved wood cellulose with a balance, soak it in 200 mL of water for 14 hours at 20 ° C, filter, and dry the filtered broad-leaved wood cellulose in a drying oven at 105 ° C for 24 hours to obtain a swollen broad-leaved wood cellulose;

[0049] Disperse 20 mg of swollen broad-leaved wood cellulose in 1224.72 mg DMSO, then add 306.18 mg of TBAH, and stir magnetically at 20°C for 2 hours at a speed of 300 r / min to obtain a broad-leaved wood with a mass concentration of 1.29 wt.%. Cellulose solution.

[0050] Adopt Fourier Transform Infrared Spectrometer (FT-IR Spectrometer) to analyze the broad-leaved wood cellulose raw material and the broad-leaved wood cellulose solut...

Embodiment 2

[0054] The broad-leaved wood cellulose solution was prepared according to the method of Example 1, the difference being that the soaking temperature was 25° C., and the soaking time was 20 h; the mass of the swollen broad-leaved cellulose was 50 mg, and the stirring time for mixing was 6 h, and the obtained The mass concentration of the hardwood cellulose solution is 3.2wt.%.

[0055] According to the method of embodiment 1, the cellulose molecular structure in the obtained broad-leaved wood cellulose solution is characterized, as figure 1 shown. figure 1 Among them, c is the FT-IR curve of the hardwood cellulose solution obtained in this example. Comparing a and c, it can be seen that the molecular structure of the cellulose in the hardwood cellulose solution obtained in this embodiment remains basically unchanged compared with the hardwood cellulose raw material, which shows that the broadleaf cellulose is in the fiber described in the present invention. It is directly dis...

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Abstract

In the present invention, the cellulose raw material is soaked in water under the condition of 15-30°C, and then dried to obtain swollen cellulose; then the cellulose is mixed with a polar organic solvent to obtain a cellulose dispersion; finally, the cellulose The dispersion liquid is mixed with the tetra-alkyl quaternary ammonium base at 15-30°C to obtain a cellulose solution, the mixing is carried out under stirring, the stirring speed is 200-400r / min, and the stirring time is 2 ~6h. The preparation method provided by the invention is to directly dissolve cellulose at 15-30°C, which can effectively inhibit the degradation of cellulose caused by high temperature conditions; and the yield of regenerated cellulose in the cellulose solution of the invention is ≥80%, indicating that The method provided by the invention can efficiently dissolve cellulose.

Description

technical field [0001] The invention belongs to the technical field of cellulose, in particular to a cellulose solution and a preparation method thereof. Background technique [0002] Cellulose is a renewable polymer material with many advantages such as easy degradation, easy modification, good biocompatibility, and low price, so it is widely used. In the process of cellulose application, the dissolution of cellulose is a technical problem, mainly because the cross-linked hydrogen bond network of cellulose molecules is extremely difficult to be destroyed, and it is difficult for conventional solvents to dissolve cellulose, which increases the difficulty of cellulose processing and is very difficult. The high-value utilization of cellulose is largely limited. [0003] At present, there are mainly two types of cellulose solvent systems, one is aqueous solvent system, and the other is non-aqueous solvent system, that is, organic solvent system. Among them, the organic solven...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/09C08L1/02
CPCC08J3/09C08J3/096C08J3/097C08J2301/02
Inventor 王飞陈晓蔡旭敏刘鑫
Owner NANJING FORESTRY UNIV
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