Method for rapidly determining content of 3-chloro-1,2-propylene glycol in PAE resin solution

A resin solution, rapid measurement technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of errors, complex time-consuming, etc., to avoid errors, improve work efficiency, and respond quickly and thoroughly.

Inactive Publication Date: 2018-02-02
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

Therefore, the extraction and derivatization processes in GC-based detection methods are not only complicated and time-consuming, but also often lead to large errors due to incomplete extraction and derivatization reactions

Method used

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  • Method for rapidly determining content of 3-chloro-1,2-propylene glycol in PAE resin solution
  • Method for rapidly determining content of 3-chloro-1,2-propylene glycol in PAE resin solution
  • Method for rapidly determining content of 3-chloro-1,2-propylene glycol in PAE resin solution

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Experimental program
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Embodiment

[0027] The present embodiment measures the MCPD content of 10 kinds of commercially available PAE resins:

[0028] (1) Sample preparation: After diluting the PAE resin sample solution 8 times, pipette 1mL into the headspace bottle accurately with a pipette gun, and then add high iodine with a concentration of 0.04mol / L and a volume of 2mL into the headspace bottle After sodium hydroxide solution, cap the headspace vial immediately, oxidize it at room temperature in the dark for 10 minutes, and inject boron with a concentration of 5 g / L (in 2 mol / L sodium hydroxide solution) and a volume of 0.8 mL with a syringe. Sodium hydride solution is enough; the PAE resin sample without redox treatment is used as blank;

[0029] (2) Establish a standard curve: Dilute the known formaldehyde standard sample after calibration into a series of solutions with a concentration gradient (1-10mmol / L), and after the redox in step (1), set the headspace sampler and gas phase The operating condition...

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Abstract

The invention belongs to the technical field of detection of pulping and papermaking chemical assistants, and discloses a method for rapidly determining the content of 3-chloro-1,2-propylene glycol ina PAE resin solution. The method comprises the following steps: diluting a PAE resin solution to be measured, sequentially adding sodium periodate for oxidation and sodium borohydride for reduction,performing head-space gas chromatography detection, recording the gas chromatography signal value of methanol, and substituting the obtained gas chromatography signal value into a pre-drafted standardcurve to obtain the content of the MCPD in the PAE resin solution sample. The method has the advantages of no preparation of toxic organic solution, no complex solvent extraction or derivatization treatment, simplicity and easiness in operation, high efficiency, objective and accurate experiment result, and good application prospect.

Description

technical field [0001] The invention belongs to the technical field of detection of chemical auxiliary agents for pulping and papermaking, and in particular relates to a method for quickly measuring the content of 3-chloro-1,2-propanediol in a PAE resin solution. Background technique [0002] Polyamide polyamine epichlorohydrin resin (PAE) is an important papermaking wet-end additive, and has been widely used in the papermaking industry due to its excellent performance. PAE is synthesized from epichlorohydrin (ECH) and polyamine oligomers, wherein the polyamine intermediate is obtained by reacting adipic acid and diethylenetriamine in aqueous solution. In order to improve the storage stability of PAE, it is necessary to adjust the pH of its solution to 3-4 with sulfuric acid or hydrochloric acid. However, the residual ECH in the reaction will be partially hydrolyzed or acidolyzed into 1,3-dichloro-2-propanol (DCP) and 3-chloro-1,2-propanediol (MCPD) in acidic medium. These...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/68
CPCG01N30/06G01N30/68
Inventor 闫宁柴欣生
Owner SOUTH CHINA UNIV OF TECH
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