A method for detecting the rubber ratio in rubber additives

By combining infrared spectroscopy with pretreatment steps, the problem of quantitative analysis of the rubber mass ratio in rubber additives was solved, achieving rapid and accurate detection results, simplifying the detection process and improving the versatility of the equipment.

CN115931763BActive Publication Date: 2026-06-02BEIJING RED AVENUE INNOVA +1

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
BEIJING RED AVENUE INNOVA
Filing Date
2022-12-30
Publication Date
2026-06-02

AI Technical Summary

Technical Problem

Existing technologies make it difficult to accurately quantify the mass ratio of rubber in rubber additives, especially in the presence of rubber carriers and dispersants. Conventional testing methods are mostly qualitative and cannot achieve accurate quantitative detection.

Method used

Infrared spectroscopy combined with pretreatment methods, including acid soaking, washing, extraction and drying steps, was used to remove impurities and interference. The absorbance values ​​of the characteristic spectral peaks of rubber in the rubber additives were measured, and the mass ratio of rubber was calculated using a standard curve.

Benefits of technology

It enables rapid and accurate detection of the mass ratio of rubber in rubber additives, simplifies the operation process, and improves the versatility of the testing equipment and the reliability of the test results.

✦ Generated by Eureka AI based on patent content.

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Abstract

This invention relates to the field of rubber additive analysis technology, and in particular to a method for detecting the rubber ratio in rubber additives. The method for detecting the rubber ratio in rubber additives of this invention includes the following steps: (A) sequentially subjecting the rubber additive to acid soaking, washing, extraction, and drying to obtain a sample to be tested; (B) using an infrared spectrometer to determine the absorbance value of the characteristic spectral peak in the sample to be tested that belongs only to a certain rubber, and calculating the absorbance ratio of the two characteristic spectral peaks; (C) using formula R... m =a×R x The formula is calculated using +b to obtain the mass ratio of rubber in the rubber additive; where a and b are the standard curve fitting coefficients, and R0 is the mass ratio of rubber in the rubber additive. m R is the mass ratio of rubber. x The absorbance ratio is given. The detection method of the present invention can quickly and accurately obtain the mass ratio of rubber in rubber additives.
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Description

Technical Field

[0001] This invention relates to the field of rubber additive analysis technology, and in particular to a method for detecting the rubber ratio in rubber additives. Background Technology

[0002] In the rubber industry, although the amount of additives used is relatively small, they play a crucial role in improving the processing and application performance of products. High-performance rubber additives can not only improve processing performance, enhance product quality, and reduce energy consumption and production costs, but also prevent aging and degradation and extend service life.

[0003] Processing aids come in various forms, including liquids, powders, and granules. Sometimes, to increase the compatibility between processing aids and rubber, sometimes to improve the dispersion performance of processing aids in rubber, and sometimes for safety and environmental protection during processing, most additive manufacturers choose to mix processing aids with rubber to produce composite additives containing rubber carriers.

[0004] Different formulation systems require different rubber carriers. Commonly used rubber carriers include natural rubber, butadiene rubber, styrene-butadiene rubber, butyl rubber, ethylene propylene diene monomer (EPDM) rubber, and ethylene-vinyl acetate copolymer, or a combination thereof. For granulation purposes, a small amount of dispersant may also be added. Commonly used dispersants include waxes, processing oils, silicone oils, inorganic fillers, fatty acids, and fatty acid derivatives.

[0005] For rubber formulation and process engineers, it is necessary to accurately know the type and amount of carrier in order to control the production process and product performance. Since the product contains a wide variety of dispersants, it is difficult to use conventional methods to qualitatively and quantitatively analyze the polymer. Currently, conventional testing methods include infrared spectroscopy and pyrolysis-gas chromatography-mass spectrometry, but they are basically only at the qualitative level.

[0006] In view of this, the present invention is hereby proposed. Summary of the Invention

[0007] The purpose of this invention is to provide a method for detecting the rubber ratio in rubber additives. After removing impurities through pretreatment, the absorbance of rubber in the rubber additives is determined by infrared spectroscopy, which can accurately analyze the mass ratio of rubber in the rubber additives.

[0008] In order to achieve the above-mentioned objectives of the present invention, the following technical solution is adopted:

[0009] This invention provides a method for detecting the rubber ratio in rubber additives, comprising the following steps:

[0010] (A) The rubber additives are subjected to acid soaking, washing, extraction and drying in sequence to obtain the sample to be tested;

[0011] (B) Using an infrared spectrometer, the absorbance values ​​of the characteristic spectral peaks in the sample to be tested that belong only to a certain rubber were measured, and the absorbance ratio of the two characteristic spectral peaks was calculated.

[0012] (C) Using formula R m =a×R x The formula is calculated using +b to obtain the mass ratio of rubber in the rubber additive; where a and b are the standard curve fitting coefficients, and R0 is the mass ratio of rubber in the rubber additive. m R is the mass ratio of rubber. x The absorbance ratio is denoted as .

[0013] Furthermore, the rubber in the rubber additive includes one or more of natural rubber, butadiene rubber, styrene-butadiene rubber, butyl rubber, ethylene propylene diene monomer (EPDM) rubber, and ethylene-vinyl acetate copolymer.

[0014] Furthermore, the acid impregnation includes adding an acid solution to the rubber additive and heating and stirring.

[0015] Preferably, the heating and stirring temperature is 60–100°C, and the heating and stirring time is 10–60 min.

[0016] Furthermore, the acid solution includes one or more of hydrochloric acid, sulfuric acid, and nitric acid.

[0017] Preferably, the concentration of the acid solution is 0.1 to 3 mol / L.

[0018] Preferably, the ratio of the acid solution to the rubber additive is 50–200 mL / g.

[0019] Furthermore, the washing includes washing with water.

[0020] Furthermore, the solvent for extraction includes one or more of alcohols, ketones, alkanes, and ethers.

[0021] Preferably, the solvent for extraction includes at least one selected from methanol, ethanol, acetone, n-hexane, n-heptane, diethyl ether, and petroleum ether.

[0022] Furthermore, the extraction includes one or more of extraction, ultrasonication, and microwave.

[0023] Furthermore, the extraction temperature is 40–80°C.

[0024] Preferably, the extraction time is 30 to 100 minutes.

[0025] Preferably, the extraction is performed 2 to 5 times.

[0026] Furthermore, the testing methods using the infrared spectrometer include one or more of the following: pellet pressing, coating, and attenuated total reflectance.

[0027] Furthermore, the method of representing absorbance includes any one of peak height, half peak height, and peak area.

[0028] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0029] The method for detecting the rubber ratio in rubber additives of the present invention involves removing impurities through a pretreatment method and then measuring the absorbance of the rubber in the rubber additive using infrared spectroscopy, which can accurately analyze and obtain the mass ratio of rubber in the rubber additive. The pretreatment method of the present invention is simple and easy to implement, and the detection equipment is a commonly used detection device that is easy to operate; the mass ratio of each rubber in the rubber additive can be obtained quickly and accurately through a simple detection method. Attached Figure Description

[0030] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0031] Figure 1 This is the standard curve of EVA / SBR in Embodiment 1 of the present invention.

[0032] Figure 2 The infrared spectra of the sample to be tested in Example 1 of this invention were measured three times.

[0033] Figure 3 This is the standard curve of EVA / NR in Embodiment 2 of the present invention.

[0034] Figure 4 This is the standard curve of SBR / NR in Embodiment 3 of the present invention. Detailed Implementation

[0035] The technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings and specific embodiments. However, those skilled in the art will understand that the embodiments described below are some embodiments of the present invention, but not all embodiments, and are only used to illustrate the present invention, and should not be regarded as limiting the scope of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall be followed. Where the manufacturers of reagents or instruments are not specified, they are all conventional products that can be purchased commercially.

[0036] The following is a detailed description of a method for detecting the rubber ratio in a rubber additive according to an embodiment of the present invention.

[0037] In some embodiments of the present invention, a method for detecting the rubber ratio in rubber additives is provided, comprising the following steps:

[0038] (A) The rubber additives are subjected to acid soaking, washing, extraction and drying in sequence to obtain the sample to be tested;

[0039] (B) Using an infrared spectrometer, the absorbance values ​​of the characteristic peaks in the sample belonging only to a certain rubber were measured, and the absorbance ratio of the two characteristic peaks was calculated.

[0040] (C) Using formula R m =a×R x The formula is calculated using +b to obtain the mass ratio of rubber in the rubber additives; where a and b are the standard curve fitting coefficients, and R0 is the standard curve fitting coefficient. m R is the mass ratio of rubber. x The absorbance ratio is denoted as .

[0041] The main component of rubber additives is the additive itself, while the rubber polymer accounts for only a small proportion. Moreover, in order to achieve composite effects and processing performance, other compounding agents such as waxes, processing oils, silicone oils, inorganic fillers, fatty acids, and fatty acid derivatives are added, making the composition of composite additives increasingly complex. This makes the detection of rubber components in rubber additives susceptible to various kinds of interference.

[0042] The method for detecting the rubber ratio in rubber additives of the present invention involves removing impurities through a pretreatment method and then measuring the absorbance of the rubber in the rubber additive using infrared spectroscopy, which can accurately analyze and obtain the mass ratio of rubber in the rubber additive. The pretreatment method of the present invention is simple and easy to implement, and the detection equipment is commonly used and easy to operate.

[0043] In some embodiments of the present invention, the rubber in the rubber additive includes one or more of natural rubber (NR), butadiene rubber (BR), styrene-butadiene rubber (SBR), butyl rubber (IIR), ethylene propylene diene monomer (EPDM), and ethylene-vinyl acetate copolymer (EVA).

[0044] In some specific embodiments of the present invention, before acid soaking, the method further includes: cutting the rubber additive into sheets.

[0045] In some embodiments of the present invention, acid immersion includes adding an acid solution to the rubber additive and heating and stirring.

[0046] In some embodiments of the present invention, the heating and stirring temperature is 60 to 100°C, and the heating and stirring time is 10 to 60 minutes; typically, but not limitingly, for example, the heating and stirring temperature is 60°C, 70°C, 80°C, 90°C, or 100°C, etc.; and the heating and stirring time is 10 minutes, 20 minutes, 30 minutes, 40 minutes, 50 minutes, or 60 minutes, etc.

[0047] In some embodiments of the present invention, the acid solution includes one or more of hydrochloric acid, sulfuric acid, and nitric acid. Preferably, the acid solution includes hydrochloric acid. Sulfuric acid and nitric acid have strong oxidizing properties, and their concentrations, if too high, can damage the polymer. Hydrochloric acid is less likely to damage the polymer.

[0048] In some embodiments of the present invention, the concentration of the acid solution is 0.1 to 3 mol / L; typically, but not limitingly, for example, the concentration of the acid solution is 0.1 mol / L, 0.5 mol / L, 1 mol / L, 1.5 mol / L, 2 mol / L, 2.5 mol / L, or 3 mol / L, etc.; preferably, the concentration of the acid solution is 0.5 to 2 mol / L.

[0049] In some embodiments of the present invention, the ratio of acid solution to rubber additive is 50–200 mL / g; typically, but not limitingly, the ratio is 50 mL / g, 100 mL / g, 150 mL / g, or 200 mL / g, etc. Preferably, the ratio is 100–200 mL / g.

[0050] In some embodiments of the present invention, washing includes water washing; preferably, the number of water washings is 2 to 10.

[0051] In some embodiments of the present invention, the extraction solvent includes one or more of alcohols, ketones, alkanes and ethers.

[0052] In some embodiments of the present invention, the extraction solvent includes at least one selected from methanol, ethanol, acetone, n-hexane, n-heptane, diethyl ether, and petroleum ether.

[0053] In some embodiments of the invention, extraction includes one or more of extraction, ultrasound, and microwave. Preferably, extraction includes ultrasound.

[0054] In some embodiments of the present invention, the extraction temperature is 40–80°C; typically, but not limitingly, the extraction temperature is 40°C, 50°C, 60°C, 70°C, or 80°C, etc.; preferably, the extraction temperature is 50–60°C.

[0055] In some embodiments of the present invention, the extraction time is 30 to 100 min; typically, but not limitingly, for example, the extraction time is 30 min, 40 min, 50 min, 60 min, 70 min, 80 min, 90 min, or 100 min, etc.

[0056] In some embodiments of the invention, the number of extractions is 2 to 5; typically, but not limitingly, the number of extractions is 2, 3, 4, or 5, etc. Preferably, the number of extractions is 3.

[0057] In some embodiments of the present invention, the drying temperature is 40–80°C and the drying time is 30–120 min.

[0058] The method for detecting the rubber ratio in rubber additives of the present invention involves first dissolving the sample by heating with acid, then washing with water to remove inorganic impurities; next, solvent extraction to remove organic impurities, obtaining an insoluble substance containing characteristic products, which is then dried and detected using an infrared spectrometer. By comparing with a standard curve, the rubber ratio in the sample can be obtained. The determination method of the present invention has the advantages of being simple, rapid, and accurate.

[0059] In some embodiments of the present invention, the method of testing with an infrared spectrometer includes one or more of the following: pellet pressing, coating, and attenuated total reflectance.

[0060] The tableting method involves mixing a dried sample and dried KBr in an agate mortar until homogeneous and thoroughly ground. The mixture is then evenly placed between the top and bottom molds of a solid tableting mold. The mold is then placed in a press and heated at 4–12 T / cm. 2 By maintaining pressure on both sides for 1 to 2 minutes, transparent or uniformly translucent ingots can be obtained. Remove the ingots, place them in a solid sample testing holder, and test them on an infrared spectrometer.

[0061] The coating method involves dissolving the sample in a solvent, applying an appropriate amount of the solution evenly onto a KBr salt plate, placing it under an infrared lamp or in a ventilated area to allow the solvent to evaporate completely, and then testing it with an infrared spectrometer. The solvent used to dissolve the masterbatch adhesive can be one or more hydrocarbons or halogenated hydrocarbons, preferably one or more of dichloromethane, trichloromethane, toluene, or tetrahydrofuran.

[0062] The ATR method involves placing the masterbatch directly under the ATR attachment for testing, using either Ge or ZnSe crystal wafers.

[0063] In some embodiments of the present invention, absorbance is expressed in the form of peak height, half-peak height, and peak area.

[0064] The infrared spectrometer used in the following examples is a Thermo Fisher Scientific 6700 infrared spectrometer.

[0065] Example 1

[0066] The method for detecting the EVA and SBR ratio in the environmentally friendly granulation accelerator provided in this embodiment includes the following steps:

[0067] (1) Sample preparation

[0068] Take 3 environmentally friendly granulation accelerator tablets (approximately 150 mg), cut them into slices with a blade, place them in a 30 mL tall weighing bottle, add 20 mL of 1 mol / L hydrochloric acid solution, heat and boil in water for 15 min, pour out the acid solution, add 20 mL of distilled water and rinse 3 times; add 30 mL of methanol, sonicate at 50 °C for 30 min, discard the methanol, add another 30 mL of methanol, repeat 3 times, place the solid sample in the weighing bottle in a 70 °C oven and heat for 45 min to obtain the sample to be tested.

[0069] (2) Preparation of standard series

[0070] Take approximately 100 mg of EVA into a 10 mL volumetric flask, dissolve and dilute to volume with toluene; take approximately 250 mg of SBR into a 25 mL volumetric flask, dissolve and dilute to volume with toluene.

[0071] Take five 5mL centrifuge tubes, add 1mL of EVA solution to each tube, and then add 1mL, 2mL, 2.5mL, 3mL, and 4mL of SBR solution respectively. Mix thoroughly and then dry in an oven at 80℃ to obtain standard samples.

[0072] (3) Test

[0073] At room temperature, the standard sample and the test sample were sequentially detected using an attenuated total reflectance-infrared spectrometer at (1240±5) cm⁻¹. -1 The absorption peak at (966±5) cm⁻¹ is the absorption peak of the O=CO structure in vinyl acetate of EVA. -1 The absorption peak at (1240±5) cm⁻¹ corresponds to the out-of-plane bending vibration of the CH group in the trans-1,4 structure of the SBR. Standard series samples were used to measure the absorption peak at (1240±5) cm⁻¹. -1 and (966±5)cm -1 Plot the absorbance ratio Rx against the corresponding EVA to SBR mass ratio Rm, fit the regression curve, and record the absorbance of the test sample at (1240±5) cm⁻¹. -1 and (966±5)cm -1 The absorbance value of the spectral peak.

[0074] (4) Calculation

[0075] The sample to be tested contains (1240±5) cm -1 and (966±5)cm -1 Substituting the absorbance ratio Rx into the following formula, the mass ratio of EVA and SBR in the sample to be tested can be calculated.

[0076] R m =a×R x +b;

[0077] In the formula, a and b are the fitting coefficients of the standard curve;

[0078] R m The mass ratio of EVA to SBR;

[0079] R x This represents the absorbance ratio of EVA to SBR.

[0080] The standard curve in this embodiment is as follows: Figure 1 As shown; the infrared spectra of the sample measured three times are as follows. Figure 2 As shown; the test results are shown in Table 1 and Table 2.

[0081] Table 1

[0082]

[0083] Table 2

[0084]

[0085] Example 2

[0086] The method for detecting the EVA and NR ratio in ZnO-80 provided in this embodiment includes the following steps:

[0087] (1) Sample preparation

[0088] Take 4 ZnO-80 tablets (approximately 200 mg), cut them into slices with a blade, place them in a 30 mL tall weighing bottle, add 20 mL of 2 mol / L hydrochloric acid solution, heat and boil in water for 10 min, pour out the acid solution, add 20 mL of distilled water and rinse 3 times; wrap the insoluble matter with a filter screen, place it in a siphon cup, add 1.5 times the volume of acetone in the siphon cup, connect the Soxhlet extraction device, reflux in water at 80 °C for 1 h, then place the filter screen in a 60 °C oven and heat for 30 min to obtain the sample to be tested.

[0089] (2) Preparation of standard series

[0090] Take approximately 100 mg of EVA into a 10 mL volumetric flask, dissolve and dilute to volume with chloroform; take approximately 250 mg of NR into a 25 mL volumetric flask, dissolve and dilute to volume with chloroform.

[0091] Take five 5 mL centrifuge tubes, add 1 mL of EVA solution to each tube, and then add 1 mL, 1.5 mL, 2 mL, 2.5 mL, and 3 mL of NR solution respectively. Mix thoroughly to obtain standard samples.

[0092] (3) Test

[0093] At room temperature, the test product was dissolved in 2 mL of chloroform, coated onto a potassium bromide window, dried with a syringe rubber bulb, and then the standard sample and the test sample were detected by infrared spectroscopy at (1240±5) cm⁻¹. -1 The absorption peak at (836±5) cm⁻¹ is the absorption peak of the O=CO structure in vinyl acetate of EVA. -1 The absorption peak at (1240±5) cm⁻¹ corresponds to the out-of-plane deformation vibration of the CH group on the cis-disubstituted carbon-carbon double bond in NR. Standard series samples were used to measure the absorption peak at (1240±5) cm⁻¹. -1 and (836±5)cm -1 Plot the absorbance ratio Rx against the corresponding EVA to NR mass ratio Rm, fit the regression curve, and record the absorbance of the test sample at (1240±5) cm⁻¹. -1 and (836±5)cm -1 The absorbance value of the spectral peak.

[0094] (4) Calculation

[0095] The sample to be tested contains (1240±5) cm -1 and (836±5)cm -1 Substituting the absorbance ratio Rx into the following formula, the mass ratio of EVA and NR in the sample to be tested can be obtained through calculation.

[0096] R m =a×R x +b;

[0097] In the formula, a and b are the fitting coefficients of the standard curve;

[0098] R m The mass ratio of EVA to NR;

[0099] R x This represents the absorbance ratio of EVA and NR.

[0100] The standard curve in this embodiment is as follows: Figure 3 As shown in the figure; the test results are shown in Tables 3 and 4.

[0101] Table 3

[0102]

[0103] Table 4

[0104]

[0105] Example 3

[0106] The method for detecting the SBR and NR ratio in R-80 provided in this embodiment includes the following steps:

[0107] (1) Sample preparation

[0108] Take 3 R-80 tablets (approximately 150 mg), cut them into slices with a blade, and place them in a 30 mL tall weighing bottle. Add 20 mL of 0.5 mol / L hydrochloric acid solution, heat to boiling in water for 30 min, pour off the acid solution, and rinse three times with 20 mL of distilled water. Add 20 mL of n-heptane, sonicate at 60 °C for 30 min, discard the n-heptane, add another 20 mL of n-heptane, and repeat three times. Place the solid sample in the weighing bottle in an oven at 80 °C and heat for 1 h to obtain the sample to be tested.

[0109] (2) Preparation of standard series

[0110] Take approximately 100 mg of SBR into a 10 mL volumetric flask, dissolve and dilute to volume with toluene; take approximately 250 mg of NR into a 25 mL volumetric flask, dissolve and dilute to volume with toluene.

[0111] Take five 5 mL centrifuge tubes, add 1 mL of SBR solution to each tube, and then add 1 mL, 1.5 mL, 2 mL, 2.5 mL, and 3 mL of NR solution respectively. Mix thoroughly to obtain standard samples.

[0112] (3) Test

[0113] At room temperature, the test product was dissolved in 2 mL of toluene, coated onto a potassium bromide window, dried with a syringe rubber bulb, and then detected by infrared spectroscopy. The results were recorded at (966±5) cm⁻¹. -1 and (836±5)cm -1 The absorbance value of the peak at that point. (966±5) cm⁻¹ -1 The absorption peak at (836±5) cm⁻¹ is the absorption peak of the out-of-plane bending vibration of CH in the trans-1,4 structure C=CH in the SBR. -1 The absorption peak at that point is the absorption peak of the out-of-plane deformation vibration of CH on the cis-disubstituted carbon-carbon double bond in NR.

[0114] (4) Calculation

[0115] The sample to be tested contains (966±5) cm -1 and (836±5)cm -1 Substituting the absorbance ratio Rx into the following formula, the mass ratio of SBR and NR in the sample to be tested can be obtained through calculation.

[0116] R m =a×R x +b;

[0117] In the formula, a and b are the fitting coefficients of the standard curve;

[0118] R m The quality ratio of SBR to NR;

[0119] R x This represents the absorbance ratio of SBR to NR.

[0120] The standard curve in this embodiment is as follows: Figure 4 As shown in the figure; the test results are shown in Tables 5 and 6.

[0121] Table 5

[0122]

[0123] Table 6

[0124]

[0125] Comparative Example 1

[0126] The detection method for the EVA and SBR ratio in the granulation accelerator provided in this comparative example is the same as in Example 1, except that the concentration of the hydrochloric acid solution is 6 mol / L.

[0127] Detection results: Due to the high concentration of hydrochloric acid, the characteristic functional groups of the polymer were destroyed during the acid boiling process. The characteristic peaks of EVA and SBR could not be clearly distinguished in the infrared spectrum, so quantitative analysis could not be performed.

[0128] Comparative Example 2

[0129] The detection method for the EVA and NR ratio in ZnO-80 provided in this comparative example is the same as that in Example 2, except that acetone of 1.5 times the volume of the siphon cup is added, the Soxhlet extraction device is connected, and the mixture is refluxed in water at 80°C for 15 minutes.

[0130] The test results for this comparative example are shown in Table 7.

[0131] Table 7

[0132]

[0133] As can be seen from Table 7, when the selected extraction time is short, the rubber ratio test results of the sample are not only not parallel, but also lower than the theoretical value.

[0134] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for detecting the rubber ratio in rubber additives, characterized in that, Includes the following steps: (A) The rubber additives were subjected to acid soaking, washing, extraction and drying in sequence to obtain the sample to be tested; The acid immersion process includes adding an acid solution to the rubber additive and heating and stirring. The heating and stirring temperature is 60~100℃, and the heating and stirring time is 10~60min; The concentration of the acid solution is 0.1~3 mol / L; The acid solution includes one or more of hydrochloric acid, sulfuric acid, and nitric acid; The ratio of the acid solution to the rubber additive is 50~200mL / g; (B) Using an infrared spectrometer, the absorbance values ​​of the characteristic spectral peaks in the sample to be tested that belong only to a certain rubber were measured, and the absorbance ratio of the two characteristic spectral peaks was calculated. (C) Using formula R m =a×R x The formula is calculated using +b to obtain the mass ratio of rubber in the rubber additive; where a and b are the standard curve fitting coefficients, R0 m R is the mass ratio of rubber. x The absorbance ratio is denoted as .

2. The method for detecting the rubber ratio in rubber additives according to claim 1, characterized in that, The rubber in the rubber additives includes one or more of the following: natural rubber, butadiene rubber, styrene-butadiene rubber, butyl rubber, ethylene propylene diene monomer (EPDM) rubber, and ethylene-vinyl acetate copolymer.

3. The method for detecting the rubber ratio in rubber additives according to claim 1, characterized in that, The washing includes washing with water.

4. The method for detecting the rubber ratio in rubber additives according to claim 1, characterized in that, The solvent used for extraction includes one or more of alcohols, ketones, alkanes, and ethers; The solvent used for extraction includes at least one of methanol, ethanol, acetone, n-hexane, n-heptane, diethyl ether, and petroleum ether.

5. The method for detecting the rubber ratio in rubber additives according to claim 1, characterized in that, The extraction includes one or more of extraction, ultrasound, and microwave.

6. The method for detecting the rubber ratio in rubber additives according to claim 1, characterized in that, The extraction temperature is 40~80℃; The extraction time is 30-100 min; The extraction is performed 2 to 5 times.

7. The method for detecting the rubber ratio in rubber additives according to claim 1, characterized in that, The methods for testing using the infrared spectrometer include one or more of the following: pellet pressing, coating, and attenuated total reflectance.

8. The method for detecting the rubber ratio in rubber additives according to claim 1, characterized in that, The absorbance can be expressed in any of the following ways: peak height, half peak height, and peak area.