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Detecting method for hydroxyl ester monomer in polycarboxylic acid slump retaining agent

A technology of hydroxyester monomer and detection method, which is applied in measurement devices, instruments, scientific instruments and other directions to achieve the effects of fast measurement speed, accurate measurement and elimination of errors

Active Publication Date: 2016-01-20
KZJ NEW MATERIALS GROUP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no relevant analytical method to test the type and content of residual hydroxyl ester monomer in polycarboxylate slump-retaining agent, so the development of qualitative and quantitative analysis and testing methods is particularly important

Method used

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  • Detecting method for hydroxyl ester monomer in polycarboxylic acid slump retaining agent
  • Detecting method for hydroxyl ester monomer in polycarboxylic acid slump retaining agent
  • Detecting method for hydroxyl ester monomer in polycarboxylic acid slump retaining agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Qualitative Analysis of Residual Hydroxyl Ester Monomer in Test Sample 1

[0042] Weigh 10 g of the sample to be tested into a 20 mL centrifuge tube, add 2 mL of ethyl acetate, shake well, and centrifuge for 10 min. The ethyl acetate supernatant was analyzed by a gas chromatograph, and the spectrum was recorded as figure 2 as shown in a. by and figure 1 Compared with the gas phase standard data of hydroxyethyl acrylate and hydroxypropyl acrylate, the residual hydroxyester monomer of this sample is analyzed to be hydroxyethyl acrylate.

Embodiment 2

[0044] Qualitative Analysis of Residual Hydroxyl Ester Monomer in Test Sample 2

[0045] Weigh 10 g of the sample to be tested into a 20 mL centrifuge tube, add 4 mL of ethyl acetate, shake well, and centrifuge for 10 min. The ethyl acetate supernatant was analyzed by a gas chromatograph, and the spectrum was recorded as figure 2 as shown in b. by and figure 1 Compared with the gas phase standard data of hydroxyethyl acrylate and hydroxypropyl acrylate, the residual hydroxyester monomer of this sample is analyzed to be hydroxypropyl acrylate.

Embodiment 3

[0047] The standard working curve is drawn from the polycarboxylate slump-retaining agent with known different hydroxyethyl acrylate content as the standard

[0048] Select polycarboxylate slump-retaining agent samples with different hydroxyethyl acrylate contents (every 25g sample contains 0.75-1.9g hydroxyethyl acrylate), accurately weigh 25g samples, add 2.0g mass concentration 32% sodium hydroxide concentrated solution alkali Solution and stir. The pH value of the sample was detected to be 14 with pH test paper. After sealing, place it at room temperature for 6 hours to obtain an alkali hydrolyzed product.

[0049] Accurately weigh 5g of the above alkali hydrolyzed product into a 10mL glass test tube, and add hydrochloric acid (1+1) dropwise until the pH of the sample is close to 7. Accurately add an appropriate amount (about 0.02g) of dimethyl sebacate, and then add ethanol to dilute to the mark to form a known sample test solution.

[0050] Adopt gas chromatography, t...

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Abstract

The invention discloses a detecting method for a hydroxyl ester monomer in a polycarboxylic acid slump retaining agent. The detecting method comprises the following steps: (1) performing qualitative detection: adopting a gas chromatographic method to acquire a gas chromatographic data of a hydroxyl ester monomer reference substance, adopting ethyl acetate to extract a polycarboxylic acid slump retaining agent sample, testing an extract liquor under the same gas chromatographic condition, and qualitatively detecting the category of the hydroxyl ester monomer in the polycarboxylic acid slump retaining agent once the retention time component consistent to the hydroxyl ester monomer appears; (2) performing quantitative detection according to the following steps: a) selecting a group of polycarboxylic acid slump retaining agent sample with known content of the hydroxyl ester monomer, performing alkaline hydrolysis and acid neutralization, and then precisely adding a defined amount of internal standard substance, dimethyl sebacate, and diluting with ethyl alcohol, thereby acquiring a group of known sample to-be-detected liquid; b) adopting a gas chromatographic method to detect the content of the alkaline hydrolysis product in the group of known sample to-be-detected liquid and drawing a standard curve; c) adopting the gas chromatographic method for detecting the content of the alkaline hydrolysis product in the to-be-detected polycarboxylic acid slump retaining agent, and seeking the corresponding content of the hydroxyl ester monomer on the standard curve.

Description

technical field [0001] The invention belongs to the technical field of building material detection, and in particular relates to a method for detecting hydroxyl ester monomers in polycarboxylic acid slump-retaining agents. Background technique [0002] Product formula analysis can provide important technical support for the development of new products and speed up product development. High performance liquid chromatography and gas chromatography are usually used to detect residual monomers (acrylic acid, methacrylic acid, maleic anhydride, etc.) to infer the monomer category of polycarboxylic acid raw materials. Hydroxyester monomers (hydroxyethyl acrylate and hydroxypropyl acrylate) are the key monomers used in polycarboxylate slump inhibitors. At present, there is no relevant analytical method to test the type and content of residual hydroxyl ester monomer in polycarboxylic acid slump retaining agent, so the development of qualitative and quantitative analysis and testing...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 郑荣平方云辉李格丽林倩
Owner KZJ NEW MATERIALS GROUP CO LTD
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