Method for detecting residual quantity of N, N-dimethyl formamide in PU (Polyurethane) leather

A technology of dimethylformamide and residue, which is applied in the field of N,N-dimethylformamide, can solve the problems of analysis error, influence of DMF detection, inability to directly detect, etc., and achieve high accuracy and easy operation Effect

Active Publication Date: 2013-12-25
JIAXING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

Choose an organic solvent to extract the residual DMF in PU leather. When extracting DMF from PU leather, the PU leather will be dissolved. In this way, the dissolved substances in PU leather may have overlapping peaks with DMF during instrument analysis, which will affect the quality of DMF. detection, causing errors to the analysis; and choosing inorganic solvent water as the extractant, because water is not applicable in many instrumental analysis, it cannot be directly detected after extraction, and it needs to be detected after back-extracting with chloroform as reported in the above-mentioned literature

Method used

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  • Method for detecting residual quantity of N, N-dimethyl formamide in PU (Polyurethane) leather
  • Method for detecting residual quantity of N, N-dimethyl formamide in PU (Polyurethane) leather

Examples

Experimental program
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Effect test

Embodiment 1

[0034] The sample used: PU leather for clothing (0.5mm thick, blue) (provided by Zhejiang Hexin Industrial Group Co., Ltd.)

[0035] 1. Detection of DMF residues in PU leather for clothing (0.5mm thick, blue)

[0036] step 1:

[0037] Weigh 5.00g of the above-mentioned PU leather sample, cut it into pieces of about 1mm×1mm in size, place it in a 100ml conical flask with a stopper, and add 55ml of N-n-butyl-N-methylimidazolium tetrafluoroethylene to the conical flask Borate ionic liquid was used as the extraction solvent, and the stopper was sealed; then the conical flask was fixed in an ultrasonic extraction apparatus, and ultrasonic extraction was performed at 70°C for 1 hour. After the extraction was completed, it was filtered to obtain the ionic liquid extract of DMF , as the sample solution to be tested.

[0038] Step 2:

[0039] (1) Prepare a blank solution:

[0040] Preparation of DMF-free PU leather samples: Cut the above PU leather into pieces of about 1mm×1mm in s...

Embodiment 2-13

[0071] According to the same detection method as in Example 1, the DMF content of the PU leather samples shown in Table 3 was detected, and the results are shown in Table 3.

[0072] Table 3: Experimental data of embodiments 2-13

[0073] Example

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Abstract

The invention relates to a method for detecting the residual quantity of N, N-dimethyl formamide in PU (Polyurethane) leather. The method comprises the following steps: S1, leaching N, N-dimethyl formamide in the PU leather by using an ionic liquid to obtain an ionic liquid extracting liquid, wherein the ionic liquid is a liquid ionic liquid at room temperature; and S2, detecting N, N-dimethyl formamide in the ionic liquid extracting liquid obtained in the S1 by using a head space capillary gas chromatography-mass spectrum combination technology so as to convert to obtain the content of N, N-dimethyl formamide in the PU leather. According to the method, the novel green solvent namely the liquid ionic liquid at room temperature is selected as the extracting agent to extract DMF (Dimethyl Formamide) in the PU leather, and the head space capillary gas chromatography-mass spectrum combination method is directly used to analyze the content of DMF in the extracting liquid, so that the detection method provided by the invention is environment-friendly, simple to operate, good in reproducibility, high in recovery rate and high in accuracy.

Description

technical field [0001] The invention relates to a method for detecting N,N-dimethylformamide (N,N-dimethylformamide, DMF) residues in leather, more specifically, relates to a method for extracting PU leather by using ionic liquid as an extractant. The residual N,N-dimethylformamide is then detected by headspace gas chromatography-mass spectrometry. Background technique [0002] PU is the abbreviation of English polyurethane, the Chinese name is polyurethane, and PU synthetic leather is polyurethane synthetic leather, which is widely used in automobiles and home interior decoration. However, DMF is widely used as a resin slurry solvent in the production process of PU synthetic leather. Although the DMF solvent has been basically removed through the steps of solvent removal, water washing, and drying in subsequent production, there are still DMF residues in the middle of the film layer, and these residual DMFs are slowly volatilized through the pores of the polymer, which not...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 张洋吴建一蔡丽玲屠晓华周志军胡丽贞洪斌汪旗
Owner JIAXING UNIV
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