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A method for characterizing the pore structure of regenerated cellulose materials

A regenerated cellulose and characterization technology, applied in the field of fiber characterization, can solve the problems of sample damage results, untrue reliability, etc.

Active Publication Date: 2019-03-01
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a new method that can truly reflect the internal pore structure of cellulose, so as to solve the problem that the existing method damages the sample and the results are not true and reliable when characterizing the internal pore structure of regenerated cellulose materials

Method used

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  • A method for characterizing the pore structure of regenerated cellulose materials
  • A method for characterizing the pore structure of regenerated cellulose materials
  • A method for characterizing the pore structure of regenerated cellulose materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1, to the characterization of the pore structure of viscose fiber

[0042] First, soak the regenerated cellulose material:

[0043] (1) Take a certain amount of viscose fiber and place it in N,N-dimethylacetamide (DMAc) solution;

[0044] (2) placed in a shaker and shaken at room temperature 25°C for 7 days;

[0045] (3) After the sample was taken out, the content of DMAc in the sample was determined to be 89% by thermogravimetric analysis.

[0046] The samples were then tested by hydrogen nuclear magnetic relaxation spectroscopy.

[0047] The CPMG pulse sequence is used in the test, the test temperature is 25°C, the echo time is 1ms, and the number of sampling points is 100.

[0048] Export the NMR relaxation data as figure 1 As shown, using the inverse Laplace formula (1), the fitting is carried out on the Matlab software.

[0049] The fitting results are as figure 2 shown.

[0050] figure 2 The abscissa in represents the logarithm of the relaxati...

Embodiment 2

[0051] Embodiment 2, the characterization of the pore structure of regenerated cellulose hydrogel

[0052] First, soak the regenerated cellulose material:

[0053] (1) Get a certain amount of cotton linter pulp (cellulose, provided by Hubei Chemical Fiber Group Co., Ltd.), dissolve the cotton linter pulp in NaOH / urea aqueous solution and let it stand to form a hydrogel, soak it in H at room temperature 2 O middle;

[0054](2) placed in a shaker and shaken at room temperature for 7 days;

[0055] (3) After the sample was taken out, it was determined by thermogravimetric analysis that the H in the sample was 2 The content of O is 85%.

[0056] The samples were then tested by hydrogen nuclear magnetic relaxation spectroscopy.

[0057] The CPMG pulse sequence is used in the test, the test temperature is 25°C, the echo time is 1ms, and the number of sampling points is 56.

[0058] Export the NMR relaxation data as image 3 As shown, using the inverse Laplace formula (1), the ...

Embodiment 3

[0061] Embodiment 3, the characterization of the hole structure of polyphosphoric acid solution regenerated fiber

[0062] First, soak the regenerated cellulose material:

[0063] (1) Get a certain amount of polyphosphoric acid solution regenerated fiber, soak in DMAc at room temperature;

[0064] (2) placed in a shaker and shaken at room temperature for 7 days;

[0065] (3) After the sample was taken out, the content of DMAc in the sample was determined to be 89% by thermogravimetric analysis.

[0066] The samples were then tested by hydrogen nuclear magnetic relaxation spectroscopy.

[0067] The CPMG pulse sequence is used in the test, the test temperature is 25°C, the echo time is 1ms, and the number of sampling points is 100.

[0068] Export the NMR relaxation data as Figure 5 As shown, using the inverse Laplace formula (1), the fitting is carried out on Matlab software.

[0069] The fitting results are as Image 6 shown.

[0070] Depend on Image 6 It can be seen...

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Abstract

The invention discloses a characterization method for a porous structure of a regenerated cellulose material. The characterization method comprises the following steps: firstly, soaking regenerated cellulose into liquid and oscillating; secondly, carrying out nuclear magnetic relaxation hydrogen spectrum test on the regenerated cellulose treated in the first step; thirdly, carrying out inverse laplace transformation on a nuclear magnetic relaxation attenuation curve obtained by the nuclear magnetic relaxation hydrogen spectrum test to obtain parameters for characterizing the porous structure of the regenerated cellulose. According to the characterization method disclosed by the invention, the relationship that relaxation time (logarithms and horizontal coordinates) is in direct proportion to the content of pores (longitudinal coordinates) can be obtained, therefore, the sizes of the pores can be qualitatively explained; if specific values of the sizes of the pores need to be determined, different formulas are adopted for calculating according to difference of samples. According to the characterization method disclosed by the invention, drying or freeze-drying treatment of samples is not needed, so original states of the samples can be well kept.

Description

technical field [0001] The invention relates to a fiber characterization method, in particular to a characterization method of the pore structure of a regenerated cellulose material. Background technique [0002] Regenerated fiber materials are widely used, and their mechanical properties are often used as one of the criteria to characterize the quality of fibers. The pore structure inside the fiber has a direct impact on the mechanical properties of the fiber. Regenerated cellulose materials are often used as fabric clothing, and their comfort and durability are related to the internal structure of regenerated cellulose. [0003] In order to improve the mechanical properties of regenerated cellulose products, it is necessary to start with its internal structure and explore the influence of internal pore structure on the mechanical properties. However, currently used pore characterization methods, such as scanning electron microscopy, nitrogen adsorption, etc., require the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N24/08
CPCG01N24/08
Inventor 张祎瑾刘瑞刚康宏亮
Owner INST OF CHEM CHINESE ACAD OF SCI
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