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Method for measuring contents of harmful organic chloride DCP (1,3-dichloro-2-propanol) of PAE (polyamide epichiorobydrin resin) wet strength agent in paper for daily use, and application of method

A technology of PAE wet strength agent and household paper, which is applied in the detection field, can solve the problems of concealing the actual risk index, high hidden dangers of operation safety, and complicated operation, so as to save the pretreatment operation, avoid the toxicity of the experiment, and the operation is simple and efficient Effect

Active Publication Date: 2019-11-19
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above reaction process, due to the incomplete reaction of polyamide polyamine and ECH in the second step, part of the monomer ECH remains, and the residual ECH is a volatile, unstable colorless oily liquid, which can be mixed with chloroform and ether It has a similar pungent smell and is moderately toxic. Animal experiments have proved that it has potential carcinogenic effects
[0004] Due to the instability of ECH, the 1,3-dichloro-2-propanol (DCP) produced by its hydrolysis or acidolysis has moderate toxicity: DCP is strongly irritating to mucous membranes, and will damage the respiratory tract after inhalation, and at the same time has anesthesia and damage to the viscera. During acute inhalation or percutaneous absorption poisoning, symptoms such as headache, dizziness, fatigue, drowsiness, nausea, vomiting, and epigastric pain will occur; in addition, ECH will also undergo hydrolysis and acidolysis to generate DCP during the reaction process, and at the same time When the polyamide polyamine reacts with ECH, the residual ECH can also enter the papermaking system, so that the ECH is hydrolyzed into DCP after being exposed to water, causing DCP to further remain in the tissue paper
In addition, with the closed recycling of papermaking white water, more and more ECH and DCP will be enriched in the white water, and these harmful substances will remain in the finished product, and will affect the health of users when they reach a certain level
[0005] At present, there is no method at home and abroad to detect the harmful organic chlorine residues of PAE wet strength agents in tissue paper; for the test of the migration of harmful organic chlorides of PAE wet strength agents with high residual risk in tissue paper, Europe and the United States There is a corresponding method in the regulations, but this method requires a derivatization pretreatment process, and many toxic chemical substances are used in the experimental method, which makes the operation of the method complicated and has high safety hazards
[0006] The Chinese patent application number 201810939356.X discloses a method and application for rapid detection of low-molecular chlorinated organics in papermaking white water. The residual amount differs by several orders of magnitude, so its detection method is not suitable for the detection of organic chlorine content in household paper. When using this method to detect the content of organic chlorine in household paper, the detection error is large, the detection limit is high, and it is easy Masking the Actual Risk Index of Organochlorinated Compounds in Tissue Paper

Method used

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  • Method for measuring contents of harmful organic chloride DCP (1,3-dichloro-2-propanol) of PAE (polyamide epichiorobydrin resin) wet strength agent in paper for daily use, and application of method
  • Method for measuring contents of harmful organic chloride DCP (1,3-dichloro-2-propanol) of PAE (polyamide epichiorobydrin resin) wet strength agent in paper for daily use, and application of method
  • Method for measuring contents of harmful organic chloride DCP (1,3-dichloro-2-propanol) of PAE (polyamide epichiorobydrin resin) wet strength agent in paper for daily use, and application of method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Example 1 Rapid Detection Method of Residues of Harmful Organic Chlorinated Compound DCP in PAE Wet Strength Agent in Tissue Paper

[0074] 1. Experimental method

[0075] (1) Sample preparation: Weigh 2.0 g of tissue paper, cut into small pieces of 5 mm × 5 mm, keep the sample as loose as possible, put it in a 20 mL headspace bottle, and press the bottle cap tightly.

[0076] (2) Solid-phase microextraction: Place the headspace vial containing the tissue sample prepared in step (1) in a manual extraction device equipped with a solid-phase microextraction needle for equilibrium adsorption. The equilibrium temperature is 45°C and the equilibrium time is 30 minutes. , adsorption for 45min.

[0077] (3) Preparation of standard solution: using water as solvent, dilute DCP standard (1,3-dichloro-2-propanol (DCP) standard, from Aladdin Reagent Co., Ltd.) to 250 mg / kg to prepare mother solution For use, add different volumes of mother liquor in the middle of 2.0g hand-sheets...

Embodiment 2

[0095] Example 2 Rapid detection method for the migratable amount of harmful organic chlorinated substance DCP of PAE wet strength agent in tissue paper

[0096] 1. Experimental method

[0097] (1) Sample preparation: Weigh 2.0g of tissue paper, cut into small pieces of 5mm×5mm, place them in a ground-mouthed conical flask with a stopper, and take 200mL of extraction solvent (distilled water and 0.9% normal saline respectively) in the Erlenmeyer flask. at 40 o C shaking water bath, extraction for 120 minutes. After standing and stratifying, take 4mL of the supernatant as the extract, put it in a 20mL headspace bottle, add 0.8g of analytically pure NaCl and press the bottle cap tightly.

[0098] (2) Solid-phase microextraction: Place the headspace bottle containing the extract prepared in step (1) in a manual extraction device equipped with a solid-phase microextraction needle for equilibrium adsorption. The equilibrium temperature is 45°C and the equilibrium time is 30 minu...

Embodiment 3

[0121] Embodiment 3 precision and accuracy experiment

[0122] The method established in Example 1 and Example 2 is used for standard addition recovery. First, 1.2 mg / kg DCP is added to the PAE-free hand-sheet as the target sample, and the method of Example 1 is used to detect the standard addition recovery of the target sample. The results are shown in Table 4 (the recovery rate of standard addition is 97.11~108.03%); followed by adding 7.5 μg / L DCP to the extract as the target sample, and the method of Example 2 is used to detect the standard recovery rate of the target sample, and the results are shown in the table 5 (the recovery rate of standard addition was 102.75-113.00%).

[0123] Table 4

[0124]

[0125] table 5

[0126]

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Abstract

The invention relates to the technical field of detection, and discloses a method for measuring contents of the harmful organic chloride DCP (1,3-dichloro-2-propanol) of a PAE (polyamide epichiorobydrin resin) wet strength agent in paper for daily use, and is used for testing the residual quantity and the migration amount of the harmful organic chloride DCP of the PAE wet strength agent in the paper for daily use through a SPME (Solid Phase Micro Extraction)-GC-MS / MS (Gas Chromatography-Tandem Mass Spectrum). The method breaks through the bottleneck that methods for detecting the contents of the harmful organic chloride of the PAE wet strength agent in the paper for daily use are not in the presence at home and abroad. Meanwhile, compared with a method for detecting the migration amount ofthe harmful organic chloride DCP of the PAE wet strength agent with a high residual risk in paper for daily use in the European Union, the method omits a pre-processing operation of derivatization, avoids test toxicity, is convenient and efficient in operation, is more suitable for the product quality control of a production process and the quick analysis of the harmful organic chloride of the PAE wet strength agent in the paper for daily use of a circulation domain and a use link.

Description

technical field [0001] The invention relates to the technical field of detection, in particular to a method for measuring the content of harmful organic chloride DCP in a PAE wet strength agent in tissue paper and an application thereof. Background technique [0002] Polyamide epichlorohydrin resin (PAE) is a commonly used wet strength agent, which is widely used in the production of facial tissues, napkins, handkerchiefs and other paper towels. [0003] PAE is a water-soluble cationic thermosetting resin, which is generally obtained through the following two-step reaction. The first step is polycondensation of dibasic acid and triamine to form polyamide polyamine, and the second step is polyamide polyamine and epoxy chloride. Propane (ECH) reacts to produce PAE resin. In the above reaction process, due to the incomplete reaction of polyamide polyamine and ECH in the second step, part of the monomer ECH remains, and the residual ECH is a volatile and unstable colorless oily...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 陈春霞武书彬程皓
Owner SOUTH CHINA UNIV OF TECH
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