CN112198078A - Method for measuring siloxane content in shoe material wear-resistant agent - Google Patents
Method for measuring siloxane content in shoe material wear-resistant agent Download PDFInfo
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- CN112198078A CN112198078A CN202011270339.5A CN202011270339A CN112198078A CN 112198078 A CN112198078 A CN 112198078A CN 202011270339 A CN202011270339 A CN 202011270339A CN 112198078 A CN112198078 A CN 112198078A
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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Abstract
The invention relates to the technical field of analysis and detection, in particular to a method for measuring the content of siloxane in a shoe material wear-resistant agent, which is characterized by comprising the following steps: weighing a proper amount of a wear-resistant agent sample, adding a proper amount of an organic solvent into a glass beaker, heating to keep micro-boiling until the sample is completely dissolved, cooling to room temperature, placing in a refrigerator for low-temperature freezing for a period of time, taking out, freezing and centrifuging, and pouring supernatant into another glass beaker; adding a proper amount of organic solvent into the remainder, repeatedly extracting supernatant for multiple times according to the first extraction method, combining the extracting solutions for multiple times, drying and weighing; the method for measuring the content of siloxane in the shoe material wear-resistant agent provided by the invention has the following beneficial effects: the invention relates to a method for measuring the content of siloxane in a shoe material wear-resisting agent, which can accurately measure the content of the siloxane as an effective component in the wear-resisting agent, thereby being capable of evaluating the excellent types of the wear-resisting agent in the market and further facilitating the material selection of the wear-resisting agent.
Description
Technical Field
The invention relates to the technical field of analysis and detection, in particular to a method for determining the content of siloxane in a shoe material wear-resistant agent.
Background
The shoe material wear-resistant agent is used for improving the performances of smoothness, glossiness, weather resistance, wear resistance, oxidation resistance, weather resistance, insulation, flame retardance and the like of the surface of the plastic sole. The wear-resistant agent is most suitable for EVA foaming middle sole and middle sole materials. At present, no related national standard, industry standard, local standard, literature report and patent related to the method for measuring the content of siloxane in the shoe material wear-resisting agent exist in China, and a blank exists in the related technical field. However, the siloxane content in the wear-resistant agents in the current market is uneven, and the dosage of the wear-resistant agents in shoe materials influences the performance of soles, so that a factory faces the problem of how to select a better wear-resistant agent, and therefore, a method for measuring the siloxane content in the wear-resistant agents of the shoe materials is urgently needed, the content of siloxane which is an effective component in the wear-resistant agents can be accurately measured, and the excellent types of the wear-resistant agents in the market can be evaluated.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and to provide a method for measuring the siloxane content in a wear-resistant agent for shoe materials, which can accurately measure the siloxane content as an active ingredient in the wear-resistant agent.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: the method for measuring the siloxane content in the shoe material wear-resisting agent is characterized by comprising the following steps of:
step 1) weighing a proper amount of wear-resistant agent sample, adding a proper amount of organic solvent into a glass beaker, heating to keep micro-boiling until the sample is completely dissolved, cooling to room temperature, placing in a refrigerator for low-temperature freezing for a period of time, taking out, freezing and centrifuging, and pouring supernatant into another glass beaker;
adding a proper amount of organic solvent into the remainder, repeatedly extracting supernatant for multiple times according to the first extraction method, combining the extracting solutions for multiple times, drying and weighing;
step 2) calculating the siloxane content of the sample according to the following formula:
wherein X is the content of siloxane in the sample;
m0 is the weight of the sample weighed in grams (g);
m1 is the weight of siloxane in grams (g) obtained after combining the multiple extracts and drying.
Preferably, the specification of the glass beaker in the step 1) is 50 mL.
Preferably, the extraction times of the extracting solution in the step 1) are two times.
Preferably, the weight of the wear-resistant agent sample weighed in the step 1) is 1-2 g.
Preferably, the weight of the anti-wear agent sample in the step 1) is weighed to be accurate to 0.0001 g.
Preferably, the organic solvent selected in step 1) is one or more of cyclohexane, n-hexane, toluene, ethyl acetate, butyl acetate and petroleum ether.
Preferably, the adding amount of the organic solvent in the step 1) is 10-30 mL.
Preferably, the low-temperature freezing temperature in the step 1) is 0-8 ℃, and the freezing time is 20-60 min.
Preferably, the temperature of the freezing centrifugation in the step 1) is 2-6 ℃, the rotating speed is 4000-10000 r/min, and the centrifugation time is 5-10 min.
As can be seen from the above description, the method for determining the siloxane content in the shoe material anti-wear agent provided by the invention has the following beneficial effects: the invention relates to a method for measuring the content of siloxane in a shoe material wear-resistant agent, which can accurately measure the content of the siloxane as an effective component in the wear-resistant agent, thereby being capable of evaluating the excellent types of the wear-resistant agent in the market and further facilitating the material selection of the wear-resistant agent; accurate measurement precision, simple operation and convenient popularization.
Drawings
Figure 1 is an infrared spectrum of a sample of the abrasion resistance agent.
FIG. 2 is an infrared spectrum of the dried two extractive solutions.
FIG. 3 is an IR spectrum of the residue after two extractions and oven drying.
Detailed Description
The invention is further described below by means of specific embodiments.
The present invention will be further described with reference to the following detailed description so that the technical means, the creation features, the achievement purposes and the effects of the present invention can be easily understood.
A method for measuring the content of siloxane in a shoe material wear-resistant agent comprises the following steps:
detailed description of the preferred embodiment 1
Weighing 1.0g (accurate to 0.0001g) of sample, adding 10mL of cyclohexane into a 50mL glass beaker, heating and keeping the sample to be slightly boiled until the sample is completely dissolved, cooling to room temperature, placing the sample in a refrigerator for freezing at 0 ℃ for 20min, taking out the sample, freezing and centrifuging at 4000r/min at 2 ℃ for 10min, pouring the supernatant into another beaker, adding 25mL of cyclohexane into the residue, repeatedly extracting once, combining the two extracting solutions, drying, weighing and calculating the siloxane content.
Specific example 2
Weighing 1.0g (accurate to 0.0001g) of sample, adding 20mL of butyl acetate into a 50mL glass beaker, heating and keeping the sample to be slightly boiled until the sample is completely dissolved, cooling to room temperature, placing the sample in a refrigerator for freezing at 4 ℃ for 40min, taking out the sample at 6000r/min at 4 ℃, freezing and centrifuging for 7min, pouring the supernatant into another beaker, adding 20mL of butyl acetate into the residue, repeatedly extracting once, combining the two extracting solutions, drying, weighing and calculating the siloxane content.
Specific example 3
Weighing 1.0g (accurate to 0.0001g) of sample, adding 10mL of n-hexane and 20mL of ethyl acetate into a 50mL glass beaker, heating and keeping the micro-boiling until the sample is completely dissolved, cooling to room temperature, placing the sample in a refrigerator for freezing at 8 ℃ for 60min, taking out the sample at 10000r/min at 6 ℃, freezing and centrifuging for 5min, pouring the supernatant into another beaker, adding 20mL of butyl acetate into the residue, repeatedly extracting once, combining the two extracting solutions, drying, weighing and calculating the siloxane content.
FIG. 1 is an infrared spectrum of a wear-resistant agent sample, FIG. 2 is an infrared spectrum of an extract obtained after two times of drying, and FIG. 3 is an infrared spectrum of a residue obtained after two times of extracting and drying. As can be seen from FIG. 3, the Si-O-Si symmetric stretching vibration absorption peak (795cm-1) of siloxane in the residue after separation had disappeared. As can be seen from fig. 2, ester group C ═ O stretching vibration absorption peak (1737cm-1) of EVA in siloxane infrared spectrogram obtained after drying the two extracting solutions is almost absent, which indicates that siloxane and EVA are basically and completely separated, and the separation effect is good, the experimental absolute error is less than 4%, and the relative error is less than 5%.
Experimental error of the method of the present invention is demonstrated by five sets of samples, with actual siloxane content of 10.0%, 25.0%, 50.0%, 75.0%, 90.0% in samples 1 to 5, respectively. The measurement results are shown in the following table 1:
TABLE 1 Experimental error of the method of the invention
| Sample (I) | Measurement of siloxane content | Actual content of siloxane | Absolute error | |
| Sample | ||||
| 1 | 9.6％ | 10.0％ | -0.4％ | -4.0％ |
| Sample 2 | 24.1％ | 25.0％ | -0.9％ | -3.6％ |
| Sample 3 | 48.8％ | 50.0％ | -1.2％ | -2.4％ |
| Sample No. 4 | 73.2％ | 75.0％ | -1.8％ | -2.4％ |
| Sample No. 5 | 86.3％ | 90.0％ | -3.7％ | -4.1％ |
The above description is only a few specific embodiments of the present invention, but the design concept of the present invention is not limited thereto, and any insubstantial modifications made by the design concept should fall within the scope of the present invention.
Claims (9)
1. The method for measuring the siloxane content in the shoe material wear-resisting agent is characterized by comprising the following steps of:
step 1) weighing a proper amount of wear-resistant agent sample, adding a proper amount of organic solvent into a glass beaker, heating to keep micro-boiling until the sample is completely dissolved, cooling to room temperature, placing in a refrigerator for low-temperature freezing for a period of time, taking out, freezing and centrifuging, and pouring supernatant into another glass beaker;
adding a proper amount of organic solvent into the remainder, repeatedly extracting supernatant for multiple times according to the first extraction method, combining the extracting solutions for multiple times, drying and weighing;
step 2) calculating the siloxane content of the sample according to the following formula:
wherein X is the content of siloxane in the sample;
m0 is the weight of the sample weighed in grams (g);
m1 is the weight of siloxane in grams (g) obtained after combining the multiple extracts and drying.
2. The method for measuring the siloxane content in the shoe material wear-resistant agent according to claim 1, characterized in that: the specification of the glass beaker in the step 1) is 50 mL.
3. The method for measuring the siloxane content in the shoe material wear-resistant agent according to claim 1, characterized in that: the extraction times of the extracting solution in the step 1) are two times.
4. The method for measuring the siloxane content in the shoe material wear-resistant agent according to claim 1, characterized in that: the mass of the wear-resistant agent sample weighed in the step 1) is 1-2 g.
5. The method for measuring the siloxane content in the shoe material wear-resistant agent according to claim 4, wherein the method comprises the following steps: in the step 1), the weight of the wear-resistant agent sample is accurately weighed to 0.0001 g.
6. The method for measuring the siloxane content in the shoe material wear-resistant agent according to claim 1, characterized in that: the organic solvent in the step 1) can be one or more of cyclohexane, n-hexane, toluene, ethyl acetate, butyl acetate and petroleum ether.
7. The method for measuring the siloxane content in the shoe material wear-resistant agent according to claim 1, characterized in that: the adding amount of the organic solvent in the step 1) is 10-30 mL.
8. The method for measuring the siloxane content in the shoe material wear-resistant agent according to claim 1, characterized in that: the low-temperature freezing temperature in the step 1) is 0-8 ℃, and the freezing time is 20-60 min.
9. The method for measuring the siloxane content in the shoe material wear-resistant agent according to claim 1, characterized in that: the temperature of the freezing centrifugation in the step 1) is 2-6 ℃, the rotating speed is 4000-10000 r/min, and the centrifugation time is 5-10 min.
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Citations (7)
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|---|---|---|---|---|
| JPH1026607A (en) * | 1996-07-11 | 1998-01-27 | Denki Kagaku Kogyo Kk | Quantitative analysis method of silicone oil |
| US5952557A (en) * | 1997-02-20 | 1999-09-14 | Nippon Sanso Corporation | Apparatus for analyzing a silicon compound gas for siloxane content |
| CN102590011A (en) * | 2011-11-22 | 2012-07-18 | 泸州北方化学工业有限公司 | Measuring method for monitoring content of siloxane in hydrochloride during organosilicone production process |
| CN102830188A (en) * | 2012-09-17 | 2012-12-19 | 通标标准技术服务(上海)有限公司 | Determining method for polydimethylsiloxane in edible oil and meat products |
| CN104181018A (en) * | 2013-05-21 | 2014-12-03 | 安捷伦科技有限公司 | Solvent Extraction Using Environmentally-Friendly Siloxane Solvents |
| CN105571999A (en) * | 2015-12-24 | 2016-05-11 | 上海微谱化工技术服务有限公司 | Analysis method of particle size of carbon black in ethylene-propylene-diene monomer (EPDM) rubber |
| CN108982717A (en) * | 2018-07-23 | 2018-12-11 | 湖北兴瑞硅材料有限公司 | The detection method of content of siloxane in a kind of organosilicon slag inclusion waste water |
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2020
- 2020-11-13 CN CN202011270339.5A patent/CN112198078A/en active Pending
Patent Citations (7)
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|---|---|---|---|---|
| JPH1026607A (en) * | 1996-07-11 | 1998-01-27 | Denki Kagaku Kogyo Kk | Quantitative analysis method of silicone oil |
| US5952557A (en) * | 1997-02-20 | 1999-09-14 | Nippon Sanso Corporation | Apparatus for analyzing a silicon compound gas for siloxane content |
| CN102590011A (en) * | 2011-11-22 | 2012-07-18 | 泸州北方化学工业有限公司 | Measuring method for monitoring content of siloxane in hydrochloride during organosilicone production process |
| CN102830188A (en) * | 2012-09-17 | 2012-12-19 | 通标标准技术服务(上海)有限公司 | Determining method for polydimethylsiloxane in edible oil and meat products |
| CN104181018A (en) * | 2013-05-21 | 2014-12-03 | 安捷伦科技有限公司 | Solvent Extraction Using Environmentally-Friendly Siloxane Solvents |
| CN105571999A (en) * | 2015-12-24 | 2016-05-11 | 上海微谱化工技术服务有限公司 | Analysis method of particle size of carbon black in ethylene-propylene-diene monomer (EPDM) rubber |
| CN108982717A (en) * | 2018-07-23 | 2018-12-11 | 湖北兴瑞硅材料有限公司 | The detection method of content of siloxane in a kind of organosilicon slag inclusion waste water |
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