Method for measuring contents of aldehyde ketone in polyether modified organosilicon
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A polyether modification, silicone technology, applied in measuring devices, instruments, scientific instruments, etc., to achieve the effects of good repeatability, simple pretreatment, high sensitivity and recovery rate
Pending Publication Date: 2021-05-04
南京美思德新材料有限公司
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Problems solved by technology
There is currently no relevant standard or method for the detection of low-molecular-weight aldehydes and ketones in raw polyether-modified silicones
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Embodiment 1
[0068] The instrument used in this experiment is a 1260 high performance liquid chromatograph from Agilent Company of the United States, equipped with a UV detector, and the wavelength of the detector is set to 360nm. The analytical column is Agilent C18 column, the model is 5um*4.6mm*250mm.
[0069] The embodiment of the present invention provides a method for measuring the content of aldehydes and ketones in polyether-modified silicone, including:
[0070] Select formaldehyde, acetaldehyde, acetone, acrolein, and propionaldehyde as the standard substances to be tested, and after accurate weighing, use chromatographic grade acetonitrile to prepare the concentrations of 0.05μg / ml, 0.1μg / ml, 0.5μg / ml, 1.0 Standard solutions of μg / ml, 1.5μg / ml, 3.0μg / ml, 5.0μg / ml, 10.0μg / ml; prepare 1% mass fraction of 2,4-dinitrophenylhydrazine solution with chromatographic grade acetonitrile, and use Chromatography-grade acetonitrile was used to prepare a 1% phosphoric acid solution.
[0071...
Embodiment 2- Embodiment 6
[0085]Detect with reference to the detection method of embodiment 1, the difference is that the polyether modified silicone sample that adopts is different, and embodiment 2 is marked as sample 2, and its molecular weight is about 1300, and embodiment 3 is marked as sample 3, and its molecular weight is about 2000, embodiment 4 is recorded as sample 4, and its molecular weight is about 3200, and embodiment 5 is recorded as sample 5, and its molecular weight is about 5000, and embodiment 6 is recorded as sample 6, and its molecular weight is about 5700, and the test results are as follows:
[0086]
[0087]
[0088] It should be noted that the samples provided in the examples of the present invention are self-made samples by the inventors, for example, sample 1 is a sample synthesized by referring to the synthesis method of document CN109942823A.
[0089] verify:
[0090] 1. Repetitive experiment
[0091] Select the polyether-modified silicone sample of Example 5 above, ...
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Abstract
The invention relates to the technical field of organosilicon polymer detection, and concretely relates to a method for measuring the content of aldehyde ketone in polyether modified organosilicon. The method comprises the following steps: carrying out a derivation reaction on to-be-detected polyether modified organosilicon and DNPH to form a reaction product; taking polyether modified organosilicon. not containing the to-be-detected polyether as a blank control, and carrying out the derivation reaction to form a blank control product; respectively detecting the reaction product and the blank control product by utilizing high performance liquid chromatography to respectively obtain peak areas of different aldehyde ketones, respectively substituting the peak areas of different aldehyde ketones into a standard curve formula of the corresponding aldehyde ketones, and calculating to respectively obtain the detection contents of the corresponding aldehyde ketones; and substituting the detected content of the corresponding aldehyde ketone into a formula to obtain the content of the aldehyde ketone corresponding to the polyether modified organosilicon to be detected, wherein the formula is as follows: W = (Ai - A0) / m. The method can effectively, accurately and quantitatively detect the content of aldehyde ketone in the polyether modified organic silicon, and is beneficial to improving the quality of the polyether modified organosilicon.
Description
technical field [0001] The invention relates to the technical field of organosilicon polymer detection, in particular to a method for determining the content of aldehydes and ketones in polyether-modified organosilicon. Background technique [0002] Silicone polymers are polymers that contain silicon elements in their molecular structure and organic functional groups are attached to silicon atoms. According to its chemical structure and performance, it can be divided into three categories: (1) silicone oil; (2) silicone rubber; (3) silicone resin. Among them, polyether-modified silicone oil is a kind of silicone non-ionic surfactant with unique performance obtained by grafting and copolymerizing polyether and dimethylsiloxane. The main uses of polyether modified silicone oil are as follows: (1) Foam stabilizer for polyurethane system foaming, making the cells fine and uniform, and the obtained products are widely used in home appliance insulation materials, automobile chair...
Claims
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