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Near-infrared spectral detection method for residual content of solvent in polyurethane elastic fiber filaments

A technology of near-infrared spectroscopy and detection methods, which is applied in the field of industrial analysis, can solve problems that have not been reported, and achieve the effects of high sensitivity, good correlation, and shortened detection cycle

Inactive Publication Date: 2015-06-24
ZHEJIANG HUAFENG SPANDEX
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of near-infrared spectroscopy to determine the content of solvent DMAC in spandex yarn in actual production has not been reported.

Method used

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  • Near-infrared spectral detection method for residual content of solvent in polyurethane elastic fiber filaments
  • Near-infrared spectral detection method for residual content of solvent in polyurethane elastic fiber filaments
  • Near-infrared spectral detection method for residual content of solvent in polyurethane elastic fiber filaments

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The establishment and application process of the near-infrared spectrum model described in the present invention are as attached figure 1 ,details as follows:

[0036] Instrument conditions and processing of spandex prepolymer samples:

[0037]Instrument: The near-infrared spectrum was collected by MB3600 Fourier transform near-infrared spectrometer of ABB company in Switzerland, which is equipped with Horizon MB analysis software, quartz liquid cell and InGaAs detector. The spectra of each sample are obtained by averaging 32 scans at a resolution of 4. The scanning range is 12000~4000cm -1 .

[0038] Sample: The sample used in the experiment is the spandex yarn collected during the spandex production process, and the extract is extracted by acetone for detection.

Embodiment 2

[0040] Sample near-infrared spectrum measurement:

[0041] In this experiment, a quartz liquid absorption cell was used. Pour different concentrations of DMAC acetone standard solutions into the liquid absorption cell, keep the temperature at 25±0.5°C, put them into the detection cell, and collect the spectrum of the sample. The same sample was scanned 32 times, according to After averaging, the final spectrogram is obtained, as shown in the attached figure 2 .

Embodiment 3

[0043] predict:

[0044] figure 2 Shown are the raw data of the spectrum, normalized and normalized, confirming 4484-5095cm -1 、5579-6167cm -1 、8212-9014cm -1 、10652-11448cm -1 The four spectral detection ranges are used as modeling bands, and the quantitative calibration model is established by segmenting using the PLS method. In order to avoid the phenomenon of "overfitting", the leave-one-out cross-validation method is used to reasonably select the number of principal factors. The number of principal factors obtained by cross-validation of the two-stage DMAC content is shown in Figure 3, and the optimal number of principal factors is 4 (0- 1.7878%, see Figure 3(a)), 5 (1.7878%-9.4362%, see Figure 3(b)).

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Abstract

The invention relates to a near-infrared spectral detection method for the residual content of a solvent N,N'-dimethylacetamide (DMAC) in polyurethane elastic fiber filaments. The method comprises the following steps: (1) preparing a series of acetone and DMAC solutions of different concentrations, and selecting a sufficient amount of representative calibration set samples; (2) determining a near-infrared spectral spectrogram of the calibration set samples, carrying out spectral pretreatment on a wave band, of 12,000-4,000cm<-1>, of the spectrogram, and then, establishing calibration models by adopting a partial least square method; (3) carrying out extracting pretreatment on the polyurethane elastic fiber filaments, then, determining a near-infrared spectral spectrogram of an extract, treating the wave band, of 12,000-4000cm<-1>, of the obtained spectrogram by adopting the same pretreatment method as in the step (2), and analyzing the pretreated spectrum by adopting the corresponding calibration model obtained in the step (2), thereby obtaining the content of DMAC in a polyurethane elastic fiber filament sample to be detected. The method has the advantages that the analysis process is simple and rapid, the interference resistance is strong, the analysis is non-destructive, the sampling quantity is small, and the like.

Description

technical field [0001] The invention relates to a near-infrared spectrum detection method for residual content of solvent N,N'-dimethylacetamide (DMAC) in spandex yarn, which belongs to the field of industrial analysis. Background technique [0002] Spandex (polyurethane) fiber is the most elastic synthetic fiber at present. It has excellent elongation at break and breaking strength. It is an indispensable special textile fiber for the production of high-grade elastic textiles. It has high application value and Good development prospects. Dry spinning is currently the most commonly used spandex production process, that is, the solution is solidified into silk due to the volatilization of the solvent under the hot air flow. Diffusion of the internal solvent to the surface is hindered by the solidified fibers on the surface, resulting in the inability of the solvent to evaporate completely and eventually forming solvent residues. DMAC is the most commonly used solvent in spa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/359
Inventor 刘珊珊钱锦李晓庆王小华薛士壮费长书朱炫相
Owner ZHEJIANG HUAFENG SPANDEX
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