Online detection method and equipment for dispersion uniformity of insoluble components

Abstract

The invention discloses an on-line detection method and equipment for dispersion uniformity of insoluble components, and the method comprises the following steps: preparing a group of test standard samples composed of insoluble components with different concentration ratios according to to-be-detected insoluble components in a to-be-detected material; detecting reflection signals of each insoluble component of the test standard sample by using an optical detection device, and establishing a multiple regression linear equation of each insoluble component of the material to be detected and light characteristics according to different reflection signals of each insoluble component to light of different wavebands; a plurality of sampling points are arranged on a material pipeline in each production stage, and an optical detection device is used for detecting reflection signals of insoluble components of the to-be-detected material at each sampling point; and calculating the concentration of each insoluble component of the to-be-detected material at each sampling point in each production stage and the dispersion non-uniformity index of each insoluble component of the to-be-detected material in each production stage according to the detected reflection signal and an established multiple regression linear equation so as to judge the dispersion uniformity of each insoluble component of the to-be-detected material in each production stage.

Description

Technical Field

[0001] The present invention relates to the technical field of on-line detection of material production, and particularly relates to an on-line detection method and device for the dispersion uniformity of insoluble components. Background Art

[0002] To improve the physical and chemical properties and mechanical properties of thermosetting resins, modifiers are usually added to the formulation. Most modifiers are insoluble in the resin matrix and are dispersed in the thermosetting resin in a "sea-island" structure. The dispersion uniformity of the modifiers has an important impact on the physical and chemical properties and mechanical properties of the resin, and is an important index that needs to be detected and controlled in industrial production.

[0003] At present, for the dispersion uniformity of mixtures, imaging methods are mostly used for detection, mainly including optical microscopes, scanning electron microscopes, transmission electron microscopes, etc., which can directly observe the states of various components in liquids or resin sections. However, the above methods can only qualitatively evaluate the dispersion uniformity of the modified components, cannot achieve quantitative detection and on-line testing of the production line, and at the same time, the above methods also have problems such as complex testing, poor representativeness, and high requirements for image contrast, and cannot provide accurate guidance for product quality control in the actual production process.

[0004] At present, there is no relevant report on the quantitative detection of the dispersion uniformity of insoluble components in the production process of thermosetting resins, and there is no relevant report on the on-line detection method for the production process. Summary of the Invention

[0005] In view of the deficiencies in the prior art, the present invention provides an on-line detection method and device for the dispersion uniformity of insoluble components, which constructs a multiple regression linear equation by using the optical characteristics of each insoluble component, uses an optical detection device to detect the reflection signal in real time during material production, and calculates the concentration of each insoluble component and the dispersion non-uniformity index of each insoluble component of the material to be tested according to the reflection signal and the multiple regression linear equation, so as to accurately and quickly quantitatively evaluate the dispersion uniformity of each insoluble component of the material to be tested, and provide strong support for quality control in the production process.

[0006] The first object of the present invention is to provide an on-line detection method for the dispersion uniformity of insoluble components, including:

[0007] According to the insoluble component to be tested in the material to be tested, a set of test standard samples composed of insoluble components with different concentration ratios is configured;

[0008] The reflection signals of each insoluble component of the test standard sample are detected by an optical detection device, and a multiple regression linear equation between each insoluble component of the material to be tested and the light characteristics is established according to the different reflection signals of each insoluble component to light of different wavelength bands;

[0009] A plurality of sampling points are provided on the material pipelines at each production stage, and an optical detection device is used to detect the reflection signals of the insoluble components of the material to be measured at each sampling point;

[0010] According to the detected reflection signals and the established multiple regression linear equation, calculate the concentrations of the insoluble components of the material to be measured at each sampling point in each production stage and the dispersion non-uniformity index of the insoluble components of the material to be measured in each production stage, so as to judge the dispersion uniformity of the insoluble components of the material to be measured in each production stage.

[0011] As a further improvement of the present invention, the configuration of a set of test reference samples composed of insoluble components with different concentration ratios includes: determining the concentration ratio step of the insoluble components according to the tolerance range of the insoluble components in the material to be measured, and configuring the test reference samples according to the concentration ratio step of the insoluble components and the concentration range of the insoluble components in the material to be measured.

[0012] As a further improvement of the present invention, according to the concentration ratio step of the insoluble components and the concentration range of the insoluble components in the material to be measured, an orthogonal test is used to form a concentration ratio matrix of the insoluble components, and the test reference samples are configured according to the concentration ratio matrix of the insoluble components.

[0013] As a further improvement of the present invention, the multiple regression linear equation of the insoluble components of the material to be measured and the optical characteristics is:

[0014]

[0015] Among them, y is an insoluble component in the material to be measured; y1 to y T is the reflection signal component of a certain component to be measured, with a total of T components; x is the reflection signal intensity of a certain component to be measured for light of different wavelength bands, x 11 ~x 1K is the reflection signal intensity of the y1 component of a certain component to be measured for light of different wavelength bands, with a total of K wavelength bands; β1 to β K is the slope constant, indicating the characteristic value of a certain insoluble component in the material to be measured at different wavelength bands; ε1 to ε T is the intercept constant, indicating the deviation of the reflection signal of a certain insoluble component in the material to be measured under different components.

[0016] As a further improvement of the present invention, according to the actual detection requirements, different numbers of sampling points can be provided on the material pipelines at each production stage, and the sampling points are provided on the material pipelines after each production stage is completed.

[0017] As a further improvement of the present invention, the material pipeline at the sampling point is a transparent pipeline, or a light-transmitting glass is provided on the material pipeline at the sampling point.

[0018] As a further improvement of the present invention, the optical detection device is composed of a light source, a signal detection module, and a signal conversion module;

[0019] The light source emits near-infrared light and visible light to the material pipeline at the sampling point;

[0020] The signal detection module receives the reflected light of the material to be measured and detects the reflection signals of the insoluble components of the material to be measured for light of different wavelength bands;

[0021] The signal conversion module converts the detected reflection signal into an electrical signal and uploads the electrical signal to the host computer;

[0022] The host computer calculates the concentrations of the insoluble components of the material to be measured at the sampling point and the dispersion non-uniformity index of the insoluble components of the material to be measured in each production stage according to the electrical signal and the multiple regression linear equation.

[0023] As a further improvement of the present invention, the calculation formula of the dispersion non-uniformity index is:

[0024]

[0025] where I is the dispersion non-uniformity index of the insoluble components of the material to be measured in each production stage, I ∈ [0, 1], y is the average value of the concentration test values of the insoluble components of the material to be measured in each production stage, and y0 is the theoretical value of the concentration of the insoluble components of the material to be measured in each production stage.

[0026] As a further improvement of the present invention, the distance between the optical detection device and the material pipeline at the sampling point is 5 cm.

[0027] The second object of the present invention is to provide an on-line detection device for the dispersion uniformity of insoluble components, which is used to implement the above on-line detection method after establishing a multiple regression linear equation between the insoluble components of the material to be measured and the light characteristics. The device includes:

[0028] Multiple optical detection devices arranged at each sampling point in each production stage, and a host computer connected to the multiple optical detection devices;

[0029] The optical detection device is used to detect the reflection signals of the insoluble components of the material to be measured at each sampling point in each production stage;

[0030] The host computer is used to calculate the concentrations of the insoluble components of the material to be measured at each sampling point in each production stage and the dispersion non-uniformity index of the insoluble components of the material to be measured in each production stage according to the reflection signals of the insoluble components of the material to be measured at each sampling point in each production stage and the multiple regression linear equation.

[0031] Compared with the prior art, the beneficial effects of the present invention are:

[0032] Construct a multiple regression linear equation using the optical properties of the insoluble components, and use an optical detection device to detect the reflection signal in real time during the production of the material. Calculate the concentration of the insoluble components and the dispersion non-uniformity index of the insoluble components in the material to be measured based on the reflection signal and the multiple regression linear equation, so as to accurately and quickly quantitatively evaluate the dispersion uniformity of the insoluble components in the material to be measured.

[0033] By detecting the dispersion uniformity of the insoluble components in the material in real time, the detection efficiency is effectively improved, and strong support is provided for quality control in the production process, facilitating the adjustment of the addition time of different components and the time of each production stage during the production process to ensure that the product quality meets the standard requirements.

[0034] The on-line detection method provided by the present invention is not only applicable to the production process of thermosetting resins, but also can be extended to the detection of the dispersion uniformity of other similar materials, and has broad market application prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 is a flowchart of the on-line detection method;

[0036] Figure 2 is a schematic diagram of the positional relationship between the optical detection device and the sampling point;

[0037] Figure 3 is a working principle diagram of the on-line detection device. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0038] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are some, but not all, of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0039] The present invention will be further described in detail below with reference to the accompanying drawings:

[0040] Please refer to Figure 1 , this embodiment provides an on-line detection method for the dispersion uniformity of insoluble components, including:

[0041] According to the insoluble components to be measured in the material to be measured, a set of test standards are configured, which are composed of insoluble components with different concentration ratios;

[0042] Use an optical detection device to detect the reflection signals of the insoluble components of the test standards. According to the different reflection signals of the insoluble components to light of different wavelength bands, establish a multiple regression linear equation between the insoluble components of the material to be measured and the optical characteristics;

[0043] A plurality of sampling points are provided on the material pipelines at each production stage, and an optical detection device is used to detect the reflection signals of the insoluble components of the material to be measured at each sampling point;

[0044] According to the detected reflection signals and the established multiple regression linear equation, calculate the concentrations of the insoluble components of the material to be measured at each sampling point in each production stage and the dispersion non-uniformity index of the insoluble components of the material to be measured in each production stage, so as to judge the dispersion uniformity of the insoluble components of the material to be measured in each production stage.

[0045] The specific steps for configuring the test reference sample are as follows:

[0046] Determine the concentration ratio step of the insoluble components according to the tolerance range of the insoluble components in the material to be measured. According to the concentration ratio step of the insoluble components and the concentration range of the insoluble components in the material to be measured, use the orthogonal experiment to form a concentration ratio matrix of the insoluble components, and configure a set of test reference samples composed of insoluble components with different concentration ratios according to the concentration ratio matrix of the insoluble components.

[0047] For example, if the tolerance range of a certain component is A±2, according to the actual equipment limitations or requirements, the concentration ratio step can be set to 1, then the concentrations of this component in the configured test reference sample are A - 2, A - 1, A, A + 1, A + 2.

[0048] Furthermore, the multiple regression linear equation of the insoluble components of the material to be measured and the optical characteristics is:

[0049]

[0050] Among them, y is an insoluble component in the material to be measured; y1~y T is the reflection signal component of a certain component to be measured, with a total of T components; x is the reflection signal intensity of a certain component to be measured for light of different wavelengths, x 11 ~x 1K is the reflection signal intensity of the y1 component of a certain component to be measured for light of different wavelengths, with a total of K wavelengths; β1~β K is the slope constant, indicating the characteristic value of an insoluble component in the material to be measured at different wavelengths; ε1~ε T is the intercept constant, indicating the deviation of the reflection signal of an insoluble component in the material to be measured at different components.

[0051] Furthermore, according to the actual detection requirements, different numbers of sampling points can be provided on the material pipelines at each production stage, and the sampling points are provided on the material pipelines after each production stage is completed; the material pipeline at the sampling point is a transparent pipeline, or a light-transmitting glass is provided on the material pipeline at the sampling point.

[0052] If the resin production process includes a mixing stage, a grinding stage, and a final product generation stage, then multiple sampling points can be set in the transportation pipeline after these three stages are completed. The spacing between the multiple sampling points set in each production stage is set according to the actual production situation.

[0053] The positional relationship between the optical detection device and the sampling point is as Figure 2 shown. Figure 2 As shown in the figure, a light-transmitting glass 11 is set on the material pipeline 1, and the optical detection device 2 is set opposite to the light-transmitting glass 11, so that the light emitted by the optical detection device can enter the material in the material pipeline 1 through the light-transmitting glass 11. Each different component in the material will reflect part of the light back into the optical detection device 2 through the light-transmitting glass 11. The distance between the optical detection device 2 and the material pipeline 1 at the sampling point is 5 cm.

[0054] Specifically, the optical detection device includes a light source, a signal detection module, and a signal conversion module;

[0055] The light source emits near-infrared light and visible light to the material pipeline at the sampling point. Part of the light is absorbed by the material to be measured, and part of the light is reflected back to the optical detection device

[0056] The signal detection module receives the reflected light of the material to be measured and detects the reflection signals of the insoluble components of the material to be measured for different wavelength bands of light;

[0057] The signal conversion module converts the detected reflection signal into an electrical signal, performs denoising processing on the electrical signal, and uploads the denoised electrical signal to the host computer;

[0058] The host computer calculates the concentrations of the insoluble components of the material to be measured at the sampling point and the dispersion non-uniformity index of the insoluble components of the material to be measured in each production stage according to the electrical signal and the multiple regression linear equation.

[0059] The calculation formula for the dispersion non-uniformity index is:

[0060]

[0061] Among them, I is the dispersion non-uniformity index of the insoluble components of the material to be measured in each production stage, I ∈ [0, 1], y is the average value of the concentration test values of the insoluble components of the material to be measured in each production stage, and y0 is the theoretical value of the concentration of the insoluble components of the material to be measured in each production stage.

[0062] The dispersion non-uniformity index reflects the gap between the test value and the theoretical value of each insoluble component. The smaller the gap, that is, the smaller |y - y0|, the smaller the I value, and the higher the dispersion uniformity of this insoluble component. The ideal situation is that the test value is equal to the theoretical value, that is, the I value is 0.

[0063] This embodiment provides an on-line detection device for the dispersion uniformity of insoluble components, which is used to implement the above on-line detection method after establishing a multiple regression linear equation between the insoluble components of the material to be measured and the optical characteristics. The device includes:

[0064] A plurality of optical detection devices arranged at each sampling point in each production stage, and a host computer connected to the plurality of optical detection devices;

[0065] The optical detection device is used to detect the reflection signals of the insoluble components of the material to be measured at each sampling point in each production stage;

[0066] The host computer is used to calculate the concentration of the insoluble components of the material to be measured at each sampling point in each production stage and the dispersion non-uniformity index of the insoluble components of the material to be measured in each production stage according to the reflection signals of the insoluble components of the material to be measured at each sampling point in each production stage and the multiple regression linear equation;

[0067] The principle of the on-line detection device is as Figure 3 shown.

[0068] The host computer transmits the calculated concentration of the insoluble components of the material to be measured at each sampling point in each production stage and the dispersion non-uniformity index of the insoluble components of the material to be measured in each production stage to the central control room, and the staff adjusts the production process according to the data displayed in the central control room, such as adjusting the addition time of different components and the time of each production stage during the production process to control the product quality.

[0069] The following verifies the effect of the on-line detection method provided by the present invention through specific experiments:

[0070] Sample: AC medium-temperature thermosetting epoxy resin (produced by AVIC Composite Materials Co., Ltd.)

[0071] The method is specifically as follows:

[0072] According to the theoretical value ranges of the components of AC medium-temperature thermosetting epoxy resin (A: 6.5% ± 1%; B: 13% ± 1%; C: 13% ± 1%), test standard samples with different concentration ratios containing three insoluble components A, B, and C are configured, where D is the matrix resin (solvent-like), and the concentration ratio step size is 0.5%. According to the orthogonal test and the concentration intervals of each component in actual production, a test standard sample matrix is formed to obtain a set of test standard samples (a total of 15), and the configuration results of the test standard samples are shown in Table 1.

[0073] Table 1

[0074]

[0075] For the test specimens numbered 1 - 13 above, an optical detection device was used for detection, and a multiple linear regression equation model was established. Test specimens numbered 14 and 15 were used to verify the accuracy of the model, and the verification data are shown in Table 2.

[0076] Table 2

[0077]

[0078] As can be seen from Table 2, the maximum absolute error of the model is 0.2%, which is less than the step size of 0.5%. Therefore, the model passes the verification.

[0079] Five sampling points were set at different positions in the three production stages of mixing, milling, and finished product respectively. The optical detection device and the established optical property model were used to test the insoluble components of the resin at the sampling points, and the test data are shown in Table 3.

[0080] Table 3

[0081]

[0082] As can be seen from Table 3, in the production process stages (mixing, milling), the dispersion uniformity of each component is greater than that in the finished product stage. The product obtained in the finished product stage is the resin for final use, and the purpose of each production stage is to make the theoretical dispersion uniformity of the components in the finished product the best. Therefore, the test results of this experiment meet the expectations.

[0083] The dispersion non-uniformity index of the insoluble components of the resin in the finished product stage was calculated, and the specific results are shown in Table 4.

[0084] Table 4

[0085] Insoluble component Resin dispersion non-uniformity index Ⅰ A 0.14 B 0.02 C 0.18

[0086] As can be seen from Table 4, the dispersion uniformity of insoluble component B is the best. The dispersion non-uniformity indices of different components in the resin are different, from which it can be seen that the dispersion uniformity of each component is related to the component characteristics. This conclusion helps to adjust the addition time of different components and the time of each production stage during the production process to control the quality of the final finished product.

[0087] Through the above embodiments, it is shown that the method provided by the present invention can quantitatively detect the concentration of insoluble components during the production process of thermosetting resins, and can calculate the dispersion non-uniformity indices of insoluble components at each stage according to the multiple linear regression equation established by the test specimens, so as to more accurately control the product quality of resins in engineering production.

[0088] The above are only the preferred embodiments of the present invention and are not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. An online detection method for the uniformity of dispersion of insoluble components, characterized in that: include: According to the insoluble components to be tested in the material to be tested, a group of test standard samples consisting of insoluble components with different concentration ratios are prepared; An optical detection device is used to detect the reflection signals of each insoluble component of the test standard sample, and a multivariate regression linear equation between each insoluble component and the optical characteristics of the test material is established according to the difference in the reflection signals of each insoluble component to light of different wavelengths; Multiple sampling points are set on the material pipeline at each production stage, and the reflection signals of the insoluble components of the material to be tested at each sampling point are detected by optical detection device; According to the detected reflection signal and the established multivariate regression linear equation, the concentration of each insoluble component of the material to be tested at each sampling point in each production stage and the dispersion heterogeneity index of each insoluble component of the material to be tested in each production stage are calculated to determine the dispersion uniformity of each insoluble component of the material to be tested in each production stage.

2. The online detection method according to claim 1, characterized in that: The configuring of a group of test standard samples consisting of insoluble components of different concentration ratios includes: determining the concentration ratio step of the insoluble components according to the tolerance range of each insoluble component in the material to be tested, and configuring the test standard samples according to the concentration ratio step of each insoluble component and the concentration range of each insoluble component in the material to be tested.

3. The online detection method according to claim 2, characterized in that: According to the concentration ratio step of each insoluble component and the concentration range of each insoluble component in the material to be tested, the concentration ratio matrix of each insoluble component is formed by orthogonalization test, and the test standard sample is configured according to the concentration ratio matrix of each insoluble component.

4. The online detection method according to claim 1, characterized in that: The multivariate regression linear equation of the insoluble components of the material to be tested and the optical properties is: Where y is an insoluble component in the material to be tested; y1~y T is the reflection signal component of a component to be measured, and there are T components in total; x is the reflection signal intensity of a component to be measured for light of different wavelengths, x 11 ~x 1K is the reflection signal intensity of the y1 component of a component to be measured to light of different bands, and there are K bands in total; β1~β K is the slope constant, which indicates the characteristic value of an insoluble component in the material to be tested in different wavelength bands; ε1~ε T is the intercept constant, which represents the deviation of the reflected signal of an insoluble component in the material to be tested under different components.

5. The online detection method according to claim 1, characterized in that: According to actual testing needs, different numbers of sampling points can be set on the material pipeline at each production stage, and the sampling points are set on the material pipeline after each production stage is completed.

6. The online detection method according to claim 5, characterized in that: The material pipeline at the sampling point is a transparent pipeline, or light-transmitting glass is arranged on the material pipeline at the sampling point.

7. The online detection method according to claim 1, characterized in that: The optical detection device is composed of a light source, a signal detection module, and a signal conversion module; The light source emits near-infrared light and visible light to the material pipeline at the sampling point; The signal detection module receives the reflected light of the material to be tested, and detects the reflected signals of the insoluble components of the material to be tested to the light of different wavelength bands; The signal conversion module converts the detected reflection signal into an electrical signal and uploads the electrical signal to the host computer; The host computer calculates the concentration of each insoluble component of the material to be tested at the sampling point and the dispersion heterogeneity index of each insoluble component of the material to be tested at each production stage based on the electrical signal and the multivariate regression linear equation.

8. The online detection method according to claim 1, characterized in that: The calculation formula of dispersion inhomogeneity index is: Among them, I is the dispersion inhomogeneity index of each insoluble component of the material to be tested at each production stage, I∈[0,1], y is the average value of the test value of the concentration of each insoluble component of the material to be tested at each production stage, and y0 is the theoretical value of the concentration of each insoluble component of the material to be tested at each production stage.

9. The online detection method according to claim 1, characterized in that: The distance between the optical detection device and the material pipeline at the sampling point is 5 cm.

10. An online detection device for the uniformity of dispersion of insoluble components, used to implement the online detection method according to any one of claims 1 to 9 after establishing a multivariate regression linear equation between each insoluble component and optical characteristic of the material to be tested, characterized in that: The device comprises: A plurality of optical detection devices arranged at each sampling point in each production stage, and a host computer connected to the plurality of optical detection devices; The optical detection device is used to detect the reflection signals of each insoluble component of the material to be tested at each sampling point in each production stage; The host computer is used to calculate the concentration of each insoluble component of the material to be tested at each sampling point in each production stage and the dispersion heterogeneity index of each insoluble component of the material to be tested at each production stage according to the reflection signal of each insoluble component of the material to be tested at each sampling point in each production stage and the multivariate regression linear equation.

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