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Method of determining impurity in acrylic acid

A technology of acrylic acid and liquid acrylic acid, which is applied in chemical method analysis, chemical instruments and methods, measuring devices, etc., and can solve problems such as monopoly of analyzers

Inactive Publication Date: 2005-11-16
MITSUBISHI CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this quantitative analysis, the detection limit of impurities is about 5 mass ppm
Setting a very specific analytical column or very specific analytical conditions can lower the detection limit to about 1 mass ppm, but this analyzer is not preferred because it will be monopolized as a proprietary analyzer

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A 20ml sample of liquid high-purity acrylic acid was weighed (20.99g), and loaded into a 50ml flat-bottomed glass test tube, and the whole was immersed in an ice bath for 15 minutes. Next in an ice bath, compress the crystallized solid in the tube at the bottom of the tube using a glass rod with a rounded flat bottom end. Then, the mother liquor remaining on top was sampled by decantation and weighed (2.02 g).

[0041] Next, the sampled mother liquor was analyzed by gas chromatography. As a gas chromatograph, GC-14A (manufactured by Shimadzu Corporation), which is generally used for analyzing normal grade acrylic acid, was used. A column with a diameter of 3 mm and a length of 1.5 m was used as the separation column. The column packing used was 15% FFAP (free fatty acid phase, available from GL Science Ltd) and 5% NPGA (neopentyl glycol adipate, available from GL Science Ltd) loaded on UNIPORTS (80-100 mesh) Acquired by GL Science Ltd.). The temperature of the colum...

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PUM

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Abstract

The present invention provides a method of quantitatively analyzing a trace amount of impurities such as furfural and benzaldehyde present in high purity acrylic acid with higher accuracy by using a conventionally used general-purpose analyzer and analysis conditions. In the present invention, a crystallized acrylic acid product and a mother liquor are obtained from liquid acrylic acid, and one of impurities in the mother liquor is quantitatively determined. Then, an amount of the impurity in the liquid acrylic acid is determined based on the determined amount of the impurity in the mother liquor and a ratio of impurity distributed to a mother liquor and to crystallized solid acrylic acid when acrylic acid is crystallized in a certain ratio.

Description

technical field [0001] The invention relates to a method for quantifying the amount of impurities in high-purity acrylic acid. The present invention more particularly relates to a method for quantifying the amount of trace impurities in high-purity acrylic acid purified from an acrylic acid solution obtained by catalytic vapor-phase oxidation of propane, propene or acrolein. Background technique [0002] Acrylic acid is important industrially as a raw material for superabsorbent polymers and as a raw material for various acrylates. The use of acrylic acid as a monomer for polymerization represented by a raw material of a superabsorbent polymer has required very high-purity acrylic acid in recent years depending on the application or function of the polymer to be formed. Accordingly, many advanced acrylic acid refining technologies have been developed and implemented industrially. [0003] Examples of these techniques include: a method involving the reaction of aldehydes su...

Claims

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Application Information

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IPC IPC(8): G01N31/00B01J20/292G01N25/14G01N30/02G01N30/04G01N30/06G01N30/54G01N30/86G01N30/88G01N33/00
CPCG01N25/147G01N2030/025
Inventor 矢田修平高崎研二铃木芳郎小川宁之
Owner MITSUBISHI CHEM CORP
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