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Esterification reagent and method for determining resin hydroxyl value

A resin and hydroxyl value technology, applied in the field of hydroxyl value detection of polymer materials, can solve the problems of long measurement process time, volatile acylation reagent, strong irritation, etc., to overcome the poor reproducibility of results, improve the working environment, The effect of reducing time

Active Publication Date: 2015-06-24
SUZHOU FIRST PV MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the above reaction needs to be refluxed at high temperature, and then needs to be cooled to room temperature to carry out acid-base titration. On the one hand, the whole measurement process takes a long time. On the other hand, the acylating reagent is volatile, resulting in poor measurement accuracy and reproducibility. ; Moreover, the acylation method uses a large amount of pyridine to dissolve the resin and participate in the reaction, and pyridine is a toxic and strongly irritating organic solvent that can damage the nervous system and internal organs, and it is listed as level 4 in the article classification table Extremely toxic substances, therefore, the use of pyridine is likely to cause harm to the health of testers and the laboratory environment

Method used

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  • Esterification reagent and method for determining resin hydroxyl value
  • Esterification reagent and method for determining resin hydroxyl value
  • Esterification reagent and method for determining resin hydroxyl value

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] The present embodiment provides a kind of method of measuring resin hydroxyl value, comprises the following steps:

[0057] (a) Prepare hydrochloric acid standard solution: Take 36 mL of concentrated hydrochloric acid and add it to a 2000 mL volumetric flask, then add ethanol to the volumetric line of the volumetric flask to make a constant volume;

[0058] (b), calibrate the concentration of hydrochloric acid standard solution: anhydrous Na 2 CO 3 Baked at 300°C for 0.5 h, accurately weighed 0.2525 g with an electronic balance and added to 50 mL of deionized water to form Na 2 CO 3 Solution, add 5 drops of bromothymol blue as an indicator, titrate with hydrochloric acid standard solution until the solution is light yellow, and this Na 2 CO 3 Boil the aqueous solution in water at 100°C until it turns blue, then add the standard hydrochloric acid solution dropwise until light yellow, cook again, repeat the operation until the color does not change after cooking, and ...

Embodiment 2

[0074] This embodiment also provides a method for measuring the hydroxyl value of the resin. The specific steps are the same as in Embodiment 1, except that the selected resin samples are different. In this example, a commercial unsaturated polyester is selected, its hydroxyl value ranges from 20 to 25, its acid value AN is 0.86 mgKOH / g, and its solid content NV% is 67.59%. The specific test and calculation results are listed in Table 2.

[0075] Resin sample acid value, solid content and measured data in the embodiment 2 of table 2

[0076]

[0077] It can be obtained that the hydroxyl values ​​measured three times for the resin sample in this embodiment are 22.43, 22.16, and 22.53 respectively, and the average value thereof is 22.37. Therefore, the hydroxyl value of the commercially available unsaturated polyester is 22.37.

Embodiment 3

[0079]This example also provides a method for measuring the hydroxyl value of the resin. The specific steps are the same as in Example 1, except that the selected resin samples are different, and the esterification reactant used is 1,6-hexamethylene diisocyanate (HDI) , the concentration of hydrochloric acid standard solution is C HCl =0.2088mol / L. In this example, a commercial saturated polyester is selected, its hydroxyl value ranges from 55 to 60, its acid value AN is 0.04236 mgKOH / g, and its solid content NV% is 59.99%. The specific test and calculation results are listed in Table 3.

[0080] Resin sample acid value, solid content and measured data in the embodiment 3 of table 3

[0081]

[0082] Thus, the three measured hydroxyl values ​​of the resin sample in this embodiment are 56.71, 56.30, and 56.42 respectively, and the average value is 56.48. Therefore, the hydroxyl value of the commercially available saturated polyester is 56.48.

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Abstract

The invention relates to an esterification reagent for determining a resin hydroxyl value and a method for determining the resin hydroxyl value by use of the esterification reagent. The esterification reagent comprises an esterification reactant and a solvent, wherein the esterification reactant is isocyanate or sulfonyl isocyanate, and the solvent is a non-alcohol pyridine-free organic solvent. The method for determining the resin hydroxyl value comprises the steps of preparation of a hydrochloric acid standard solution, calibration of the concentration of the hydrochloric acid standard solution, calculation of the hydroxyl value of a resin sample, and the like. Active isocyanate or sulfonyl isocyanate serving as an esterification reactant and the hydroxyl of resin can perform a quantitative esterification reaction at room temperature, so that the method is suitable for determining the hydroxyl value of the hydroxyl-containing resin with deep color and high viscosity; moreover, a pyridine-free non-alcohol organic solvent can be adopted, thereby being more environment-friendly; due to the reaction at room temperature, the method for determining the resin hydroxyl value by use of the esterification reagent greatly reduces the reaction difficulty, shortens the required time of the reaction, and overcomes the shortcomings of low result reproducibility and the like caused by the volatilization of the esterification reagent at high temperature; moreover, the method eliminates the pollution of pyridine so as to effectively improve the working environment.

Description

technical field [0001] The invention belongs to the field of hydroxyl value detection of polymer materials, and in particular relates to an esterification reagent for measuring the hydroxyl value of resin and a method for measuring the hydroxyl value of resin by using the esterification reagent. Background technique [0002] At present, acetic anhydride acylation method and phthalic anhydride acylation method are commonly used in industrial production and scientific research to measure the hydroxyl value of resins. Ⅰ), then titrate the acid generated by the hydrolysis of excess acid anhydride with alkaline standard solution, and calculate the hydroxyl value from the titration difference between the sample to be tested and the blank test solution. [0003] (I) [0004] However, the above reaction needs to be refluxed at high temperature, and then needs to be cooled to room temperature to carry out acid-base titration. On the one hand, the whole measurement process takes a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N31/16
Inventor 张宇辉汤建成杨楚峰李勋
Owner SUZHOU FIRST PV MATERIAL CO LTD