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Method for measuring trace hydroxyl value of modified polyphenyl ether

A determination method and polyphenylene ether technology, applied in the field of detection, can solve the problems of titration hydroxyl value, no detection process, quantitative analysis of difficult phenolic hydroxyl groups, etc., and achieve short detection time, broad prospects and practical value, and high detection precision. Effect

Inactive Publication Date: 2022-02-01
ZHUHAI HONGCHANG ELECTRONICS MATERIAL
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0003] However, due to the limitation of the degree of reaction, there are often traces of terminal hydroxyl groups that cannot be reacted during the modification process, and its value has a direct impact on the dielectric properties of the modified polyphenylene ether, so it has a great influence on the remaining Quantitative analysis of phenolic hydroxyl value is necessary
However, because the modified polyphenylene ether is insoluble in water and alcohols, it is difficult to titrate the hydroxyl value by conventional acid-base titration; at the same time, because the hydrogen atom on the phenolic hydroxyl group is an active hydrogen, the peak area in the H NMR spectrum is related to the proton No quantitative relationship, it is difficult to directly carry out quantitative analysis of phenolic hydroxyl content
Moreover, the large-scale industrial application of modified polyphenylene ether in 5G polymers has occurred in the past five years. At present, there is no relevant detection technology. If a detection method for trace hydroxyl value in 5G modified polyphenylene ether can be developed, and Cross-validation with existing products has important guiding significance for the development of more modified polyphenylene ethers with excellent performance

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  • Method for measuring trace hydroxyl value of modified polyphenyl ether
  • Method for measuring trace hydroxyl value of modified polyphenyl ether
  • Method for measuring trace hydroxyl value of modified polyphenyl ether

Examples

Experimental program
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Effect test

Embodiment 1

[0038] (1) Modified polyphenylene ether fluorination

[0039] Add 0.5 g of dried modified polyphenylene ether HC P45 sample (Zhuhai Hongchang Electronic Materials Co., Ltd., Zhuhai, China) into a 10 ml injection bottle, add 5 mg of potassium carbonate powder and 3 ml of anhydrous chloroform, and stir to dissolve. Inject about 6.46mg of 3,3,3-trifluoropropionyl chloride (CAS No.41463-83-6) with a needle, the molar ratio of modified polyphenylene ether HC P45 to trifluoropropionyl chloride is about 1:5, and stir magnetically at room temperature Response 15mins. After the reaction is complete, add 20ml of methanol solution, wait for solids to precipitate, remove the solvent by suction filtration, and repeat washing three times to obtain fluorinated modified polyphenylene ether powder, which can be dried in a vacuum oven at 40°C overnight to obtain fluorinated modified polyphenylene ether . The fluorination reaction formula is as figure 2 .

[0040] (2) NMR sample preparation...

Embodiment 2

[0047] (1) Modified polyphenylene ether fluorination

[0048] Add 0.5 g of dried modified polyphenylene ether HC P45 sample (Zhuhai Hongchang Electronic Materials Co., Ltd., Zhuhai, China) into a 10 ml injection bottle, add 5 mg of potassium carbonate powder and 3 ml of anhydrous chloroform, and stir to dissolve. Inject about 6.46mg of 3,3,3-trifluoropropionyl chloride with a needle, the molar ratio of modified polyphenylene ether HC P45 to trifluoropropionyl chloride is about 1:5, and react with magnetic stirring at room temperature for 30mins. After the reaction is complete, add 20ml of methanol solution, wait for solids to precipitate, remove the solvent by suction filtration, and repeat washing three times to obtain fluorinated modified polyphenylene ether powder, which can be dried in a vacuum oven at 40°C overnight to obtain fluorinated modified polyphenylene ether .

[0049] (2) NMR sample preparation and detection

[0050] Weigh 44.09 mg (accurate to 0.01 mg) of the ...

Embodiment 3

[0056] (1) Modified polyphenylene ether fluorination

[0057] Add 0.5 g of dried modified polyphenylene ether Sabic SA 9000 sample (SABIC, Saudi Arabia) into a 10 ml injection bottle, add 5 mg of potassium carbonate powder and 3 ml of anhydrous chloroform, and stir to dissolve. Inject about 8.58mg of 2,4,5-trifluorobenzoyl chloride (CAS No.88419-56-1) with a needle, and the molar ratio of modified polyphenylene ether Sabic SA9000 to 2,4,5-trifluorobenzoyl chloride is about 1 : 5, magnetic stirring reaction at room temperature for 15mins. After the reaction is complete, add 20ml of methanol solution, wait for solids to precipitate, remove the solvent by suction filtration, and repeat washing three times to obtain fluorinated modified polyphenylene ether powder, which can be dried in a vacuum oven at 40°C overnight to obtain fluorinated modified polyphenylene ether .

[0058] (2) NMR sample preparation and detection

[0059] Weigh 52.42 mg of fluorinated modified polyphenylen...

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Abstract

The invention provides a method for determining a trace hydroxyl value of modified polyphenyl ether, and relates to the technical field of detection. The method comprises the following steps of carrying out fluorination reaction: dissolving the modified polyphenyl ether to be determined in an organic solvent, adding an acid-binding agent and a fluorination reagent, carrying out fluorination end-capping reaction, purifying after the reaction is finished, and removing the organic solvent and the unreacted fluorination reagent to obtain fluorinated modified polyphenyl ether; performing nuclear magnetic detection: taking the fluorinated modified polyphenyl ether, adding an internal standard substance and a deuterated solvent, dissolving to obtain a nuclear magnetic detection sample, and performing 19F-NMR quantitative detection; analyzing and calculating: acquiring the peak area of the fluorinated modified polyphenyl ether in the nuclear magnetic resonance fluorine spectrum chemical shift of -63.61 to -63.67 ppm, and calculating according to the formula 1 and the formula 2 to obtain the phenolic hydroxyl group value W (OH) of the modified polyphenyl ether to be measured. The method provided by the invention can accurately and rapidly measure the trace hydroxyl value of the modified polyphenyl ether.

Description

technical field [0001] The invention relates to the technical field of detection, in particular to a method for measuring the trace hydroxyl value of modified polyphenylene ether, especially for the method for measuring the trace hydroxyl value of modified polyphenylene ether applied to 5G. Background technique [0002] Polyphenylene ether is a high-performance thermoplastic resin with excellent comprehensive properties. It is widely used in the fields of communication and electronics because of its excellent dielectric properties. In recent years, with the rapid development of 5G (The Fifth Generation) communication technology, higher requirements have been placed on the performance of dielectric materials. Polyphenylene ether is an important part of the resin system of high-frequency and high-speed copper clad laminate substrate materials, but most of them are difficult to meet the requirements of processing and heat resistance. At present, manufacturers at home and abroa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N24/08G01N1/28
CPCG01N24/085G01N24/088G01N1/28
Inventor 江胜宗林仁宗袁青青
Owner ZHUHAI HONGCHANG ELECTRONICS MATERIAL
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