Sample particle dispersing system and method and laser particle analyzer equipment

Abstract

The invention provides a sample particle dispersion system and method and laser particle analyzer equipment, and belongs to the field of sample particle dispersion. The sample particle dispersing system comprises a dispersing unit, a recycling unit and a conveying unit, the dispersing unit is used for dispersing sample particles to obtain a mixed solution of the sample particles and a dispersing agent, the sample particles are solid particles for particle size analysis, and the dispersing agent is an organic solvent for dispersing the sample particles; the recycling unit is connected with the dispersing unit and is used for filtering the mixed solution to obtain a recycled solution of the dispersing agent; the conveying unit is respectively connected with the dispersing unit and the recycling unit, and the conveying unit is used for conveying the recycling liquid of the dispersing agent to the dispersing unit for one or more times. According to the technical scheme, the dispersing agent can be recycled, the consumption of the dispersing agent and the waste liquid treatment cost are reduced, and meanwhile the accuracy of the analysis result of the laser particle analyzer is guaranteed.

Description

Technical Field

[0001] The invention relates to the field of sample particle dispersion, and in particular to a sample particle dispersion system, method and laser particle size analyzer equipment. Background Art

[0002] At present, the global production capacity and demand for compounds are increasing. While mass production is in progress, the performance requirements for compounds are also getting higher and higher. For some polymer compounds, particle size distribution is an important reference indicator. At present, laser particle size analyzers are mostly used to analyze the particle size of sample particles. In order to obtain more accurate particle size data, it is usually necessary to disperse the sample particles.

[0003] However, most laser particle size analysis equipment is usually manually operated and lacks an automated dispersion system. The test is cumbersome and time-consuming. At the same time, the handling and recovery of the dispersant are not considered, resulting in waste of the dispersant. Summary of the invention

[0004] The purpose of the present invention is to provide a sample particle dispersion system, method and laser particle size analyzer equipment, which are used to solve the problem of dispersant treatment and recovery in the sample particle dispersion system.

[0005] In order to achieve the above-mentioned purpose, the present invention provides a sample particle dispersion system, including a dispersion unit, a recovery unit and a conveying unit, wherein the dispersion unit is used to disperse the sample particles to obtain a mixed liquid of the sample particles and a dispersant, the sample particles are solid particles for particle size analysis, and the dispersant is an organic solvent for dispersing the sample particles; the recovery unit is connected to the dispersion unit, and the recovery unit is used to filter the mixed liquid to obtain a recovered liquid of the dispersant; the conveying unit is respectively connected to the dispersion unit and the recovery unit, and the conveying unit is used to convey the recovered liquid of the dispersant to the dispersion unit once or multiple times.

[0006] In some embodiments, a first switch valve is provided between the dispersion unit and the recovery unit, and the first switch valve is used to control the outflow of the mixed liquid when it is opened.

[0007] In some embodiments, the dispersion unit includes a dispersion cup and a disperser, wherein the dispersion cup is used to contain sample particles and a dispersant; and the disperser is used to disperse the sample particles to obtain a mixed solution.

[0008] In some embodiments, the dispersion unit further includes a glove box, and the dispersion cup is placed inside the glove box. The glove box is used to keep the operating environment of the dispersion cup in a closed state.

[0009] In some embodiments, the recovery unit includes a filtering module and a storage module, wherein the filtering module is used to filter the mixed liquid to obtain the recovered liquid of the dispersant; and the storage module is used to store the recovered liquid of the dispersant.

[0010] In some embodiments, the storage module includes a liquid storage tank and a vacuum pump, wherein the liquid storage tank is used to store dispersant and recovered liquid of the dispersant, and the liquid storage tank is provided with a liquid replenishing port, which is used to add dispersant when the liquid storage capacity in the liquid storage tank is lower than a preset liquid storage capacity threshold; the vacuum pump is used to extract air in the liquid storage tank to form a vacuum environment.

[0011] In some embodiments, the system further includes a control unit, the delivery module includes a peristaltic pump, and the control unit is used to control the delivery of a quantitative amount of dispersant by adjusting the pipeline cross-sectional area, flow rate and single delivery time of the peristaltic pump.

[0012] In a second aspect, the present invention also provides a sample particle dispersion method, the method comprising: mixing sample particles and a dispersant to obtain a mixed solution of the sample particles and the dispersant; filtering the mixed solution to obtain a recovered solution of the dispersant; and using the recovered solution of the dispersant to prepare a mixed solution.

[0013] In a third aspect, the present invention further provides a laser particle size analyzer device, which includes a laser particle size analyzer and the above-mentioned sample particle dispersion system, and the laser particle size analyzer is used to detect a mixture of sample particles and a dispersant.

[0014] In some embodiments, the sample particles are polyolefin catalysts.

[0015] The beneficial effects of the present invention are as follows: through the above technical solution, the dispersant can be recycled, the consumption of the dispersant and the cost of waste liquid treatment can be reduced, and the accuracy of the analysis result of the laser particle size analyzer is guaranteed.

[0016] Other features and advantages of the embodiments of the present invention will be described in detail in the subsequent detailed description. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] The accompanying drawings are used to provide a further understanding of the embodiments of the present invention and constitute a part of the specification. Together with the following specific implementations, they are used to explain the embodiments of the present invention, but do not constitute a limitation on the embodiments of the present invention. In the accompanying drawings:

[0018] Figure 1 is a block diagram of a sample particle dispersion system according to an embodiment of the present invention;

[0019] Figure 2 is a schematic diagram of a sample particle dispersion system according to an embodiment of the present invention;

[0020] Figure 3 FIG. 4 is a flow chart of a sample particle dispersion method according to an embodiment of the present invention. DETAILED DESCRIPTION

[0021] The specific implementation of the embodiment of the present invention is described in detail below in conjunction with the accompanying drawings. It should be understood that the specific implementation described here is only used to illustrate and explain the embodiment of the present invention, and is not used to limit the embodiment of the present invention.

[0022] Figure 1 1 is a block diagram 100 of a sample particle dispersion system according to an embodiment of the present invention. Figure 1 As shown, the system 100 includes a dispersion unit 101, a recovery unit 102 and a conveying unit 103, wherein the dispersion unit 101 is used to disperse sample particles to obtain a mixed solution of sample particles and a dispersant, the recovery unit 102 is connected to the dispersion unit 101, and is used to filter the mixed solution to obtain a recovered solution of the dispersant, and the conveying unit 103 is respectively connected to the dispersion unit 102 and the recovery unit 103, and is used to convey the recovered solution of the dispersant to the dispersion unit 101 once or multiple times.

[0023] It should be noted that when using a laser particle size analyzer to test the particle size of sample particles, in order to obtain accurate particle size data, the agglomerated particles need to be opened to form particle monomers uniformly dispersed in the dispersant. The above-mentioned sample particles are solid particles for particle size analysis, and the dispersant is an organic solvent for dispersing the sample particles.

[0024] Generally speaking, if water is used as a dispersant, there is no need to consider the treatment and recovery of the dispersant, but for some samples that are easily soluble in water, other organic solvents need to be used as dispersants. For example, for polyolefin catalysts, it is necessary to select an organic solvent hexane as a dispersant, and the dispersant hexane used by the laser particle size analyzer is mostly used once, resulting in a waste of resources, or precipitation and reuse, affecting the accuracy of the analysis, or artificial filtration and reuse causing health damage and environmental pollution. Therefore, the technical solution provided by the embodiment of the present invention can treat and recycle the dispersant of the organic solvent, can realize the recycling of the dispersant, reduce the consumption of the dispersant and the cost of waste liquid treatment, and at the same time ensure the accuracy of the analysis results of the laser particle size analyzer.

[0025] In some embodiments, a first switch valve is provided between the dispersion unit 101 and the recovery unit 102, wherein the first switch valve is used to control the outflow of the mixed liquid when it is opened. Preferably, the first switch valve may be a solenoid valve.

[0026] In some embodiments, the dispersion unit 101 may include a dispersion cup and a disperser, wherein the dispersion cup may be used to contain sample particles and a dispersant, and the disperser may be used to disperse the sample particles to obtain the mixed solution.

[0027] In some embodiments, the dispersion unit 101 further includes a glove box, and the dispersion cup is placed inside the glove box. The glove box is used to keep the operating environment of the dispersion cup in a closed state.

[0028] It should be noted that during the mixing process of sample particles and dispersants, since some dispersants are volatile harmful solvents, placing a dispersion cup in a glove box allows the operator to operate and handle items in a completely closed state, effectively preventing environmental pollution.

[0029] In some embodiments, the recovery unit 102 may include a filtering module and a storage module, wherein the filtering module is used to filter the mixed liquid to obtain the recovered liquid of the dispersant, and the storage module is used to store the recovered liquid of the dispersant.

[0030] It is understandable that when the laser particle size analyzer performs particle size analysis on sample particles, the amount of sample particles required is extremely small. Therefore, when the filtration module filters the mixed liquid, the sample particles can be filtered on the filter paper or filter screen in the filtration module. The operator needs to regularly replace the filter paper or clean the filter screen to ensure the recovery rate of the dispersant next time.

[0031] In some embodiments, the above-mentioned storage module may include a liquid storage tank and a vacuum pump, wherein the liquid storage tank is used to store dispersant and dispersant recovery liquid, the liquid storage tank is provided with a liquid replenishing port, and the liquid replenishing port is used to add dispersant when the liquid storage capacity in the liquid storage tank is lower than a preset liquid storage capacity threshold, and the vacuum pump is used to extract air in the liquid storage tank to form a vacuum environment.

[0032] In the embodiment of the present invention, a certain amount of blank space is left in the liquid storage tank to ensure that the vacuum pump does not suck back the stored liquid. The above-mentioned vacuum pump is mainly used to maintain the storage environment of the dispersant in the liquid storage tank and to extract the mixed liquid into the integrated filtering liquid storage tank. There is no specific limitation on this, and it can also be a nitrogen pump or other equipment that can maintain the storage environment.

[0033] In some embodiments, the sample particle dispersion system may further include a control unit, and the delivery module may include a peristaltic pump, wherein the control unit may be used to control the delivery of a quantitative amount of dispersant by adjusting the pipeline cross-sectional area, flow rate, and single delivery time of the peristaltic pump.

[0034] In an embodiment of the present invention, the control unit can also be used to control the first switch valve and the vacuum pump, for example, by controlling the opening and closing time of the first switch valve to control the outflow of the dispersant, and controlling the single opening time of the vacuum pump to extract the air in the liquid storage tank.

[0035] For ease of understanding, the above sample particle dispersion system is illustrated below with reference to an example.

[0036] Figure 2is a schematic diagram of a sample particle dispersion system according to an embodiment of the present invention. Figure 2 As shown, the sample particle dispersion system may include: a dispersion cup 1, a solenoid valve 2, an integrated filter liquid storage tank 3, a vacuum pump 4, a peristaltic pump 5, a disperser 6, a PLC 7, and a tee 8, wherein the dispersion cup 1 and the disperser 6 may constitute a dispersion unit, the integrated filter liquid storage tank 3 and the vacuum pump may constitute a recovery unit, and the peristaltic pump may constitute a conveying unit. The solenoid valve 2 may be disposed between the dispersion cup 1 and the integrated filter liquid storage tank 3, and connected to one end of the tee 8, and the other two ends of the tee 8 may be respectively connected to the dispersion cup 1 and the integrated filter liquid storage tank 3, so that the overflow liquid and the mixed liquid in the dispersion cup 1 may be combined and flow out into the integrated filter liquid storage tank 3. In the embodiment of the present invention, the vacuum pump 4, the peristaltic pump 5, and the solenoid valve 2 are all anti-corrosion and explosion-proof, and the above-mentioned components may be connected by a connecting pipe, wherein the material of the connecting pipe is not reactive with the dispersant and is not easily corroded. In some embodiments, the sample particles may be a polyolefin catalyst, the dispersant may be hexane, the dispersion cup 1 and the integrated filter storage tank 3 may be 304 stainless steel, the connecting pipe may be polyethylene, and the tee 8 may be polytetrachloroethylene. This is only an example of the various components of the sample particle dispersion system and is not a further limitation of the present invention.

[0037] See also Figure 2 , the operator can add the sample particles into the dispersion cup 1 in the glove box (the glove box includes components such as dispersion cups that require manual operation, and the glove box is not indicated in the figure). After the sample particles are added into the dispersion cup 1, PLC7 controls the peristaltic pump 5 to input an appropriate amount of dispersant into the dispersion cup 1 (the dispersion cup 1 is provided with an opening at a certain distance from the cup mouth, which is connected to the tee 8, which is used to overflow when too much dispersant flows in, to prevent the dispersant from splashing to the outside of the dispersion cup 1 and polluting the operating environment), and the disperser 6 is turned on to disperse the sample particles and dispersant in the dispersion cup 1 so that the sample particles and the dispersant are evenly mixed. After the sample particles are dispersed, a mixed liquid of the sample particles and the dispersant is obtained, and part of the mixed liquid is controlled to flow into the laser particle size analyzer (the laser particle size analyzer is connected to the dispersion cup 1, not indicated in the figure), and the laser particle size analyzer is used to analyze the sample particles. After the particle size analysis, PLC7 controls the opening of the solenoid valve 2 (at this time, in order to allow the sample particles to flow out fully, PLC7 can also control the peristaltic pump 5 to input a small amount of dispersant multiple times to take away the residues of the sample particles in the dispersion cup 1, so as to complete the cleaning of the dispersion cup 1), and the mixed liquid flows into the integrated filter liquid storage tank 3 through the solenoid valve 2. The integrated filter liquid storage tank 3 is provided with a filter module and a storage module, which can filter the mixed liquid to obtain the recovered liquid of the dispersant, and store the recovered liquid of the dispersant in the liquid storage tank. The PLC controls the vacuum pump 4 to extract the air in the liquid storage tank to extract the mixed liquid into the integrated filter liquid storage tank while maintaining the vacuum to maintain the performance of the dispersant.

[0038] It should be noted that the above-mentioned integrated filter liquid storage tank 3 initially stores a certain capacity of dispersant, which can meet 5 to 10 times the single dispersion inflow. After the peristaltic pump 5 adds the dispersant in the integrated filter liquid storage tank 3 into the dispersion cup 1, the sample particle dispersion system of the present invention can realize the secondary utilization of the dispersant. However, due to the loss caused by the volatilization of the dispersant during the sample making and filtration process, the recovered liquid of the dispersant will be less. Since a certain amount of dispersant is required for each sufficient dispersion of the sample particles, when the storage capacity in the integrated filter liquid storage tank is lower than the preset storage capacity threshold, the dispersant needs to be manually added.

[0039] Figure 3 FIG. 1 is a flow chart of a sample particle dispersion method according to an embodiment of the present invention. Figure 3 As shown, the method includes the following steps.

[0040] Step S11, mixing sample particles and a dispersant to obtain a mixed solution of the sample particles and the dispersant.

[0041] It should be noted that the sample particles are solid particles for particle size analysis, and the dispersant is an organic solvent for dispersing the sample particles.

[0042] Step S12, filtering the mixed solution to obtain a dispersant recovery solution.

[0043] Step S13, using the recovered liquid of the dispersant to prepare a mixed liquid.

[0044] The sample particle dispersion method provided by the embodiment of the present invention realizes the recycling of the dispersant, and the recycled dispersant can still be used for the next dispersion without affecting the test result of the laser particle size analyzer.

[0045] An embodiment of the present invention further provides a laser particle size analyzer device, which includes a laser particle size analyzer and the sample particle dispersion system described above in the present application, wherein the laser particle size analyzer is used to detect a mixture of sample particles and a dispersant.

[0046] In some embodiments, the sample particles are polyolefin catalysts.

[0047] In order to further verify that the recovery liquid of the dispersant of the laser particle size analyzer device provided in the embodiment of the present invention does not affect the particle size analysis test of the sample particles, the inventors conducted experiments using a variety of sample particles and obtained the test results shown in Table 1.

[0048] Table 1 Test results

[0049]

[0050]

[0051] Among them, it needs to be explained that D50 is a common particle size index used to describe the particle size of a particle object. D50 represents the median particle size (in μm) that divides the particle into two parts when the particle object is distributed by mass or volume. RSD (Relative Standard Deviation) refers to relative standard deviation, which is a statistical indicator used to measure the degree of variation in a data set. It is calculated by dividing the standard deviation by the mean and is usually expressed as a percentage.

[0052] As shown in Table 1, the relative standard deviation of D50 of the laser particle size analyzer provided by the embodiment of the present invention is less than 5% compared with the original method. That is, the laser particle size analyzer provided by the embodiment of the present invention adopts the above-mentioned sample particle dispersion system to achieve the filtration and reuse of the dispersant, and the filtration accuracy meets the method requirements, reduces the uncertainty factors caused by manual operation, reduces environmental pollution and the operator's operation risk, and at the same time, realizes the automation of the dispersion process and shortens the test time.

[0053] It should also be noted that the terms "include", "comprises" or any other variations thereof are intended to cover non-exclusive inclusion, so that a process, method, commodity or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, commodity or device. In the absence of more restrictions, the elements defined by the sentence "comprises a ..." do not exclude the existence of other identical elements in the process, method, commodity or device including the elements.

[0054] The above are only embodiments of the present application and are not intended to limit the present application. For those skilled in the art, the present application may have various changes and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included within the scope of the claims of the present application.

Claims

1. A sample particle dispersion system, characterized in that: The system comprises a dispersion unit, a recovery unit and a conveying unit, wherein: The dispersing unit is used to disperse sample particles to obtain a mixed solution of the sample particles and a dispersant, the sample particles are solid particles for particle size analysis, and the dispersant is an organic solvent for dispersing the sample particles; The recovery unit is connected to the dispersing unit, and the recovery unit is used to filter the mixed liquid to obtain a recovery liquid of the dispersant; The conveying unit is connected to the dispersing unit and the recovery unit respectively, and is used to convey the recovery liquid of the dispersant to the dispersing unit once or multiple times.

2. The system according to claim 1, characterized in that A first switch valve is provided between the dispersion unit and the recovery unit, and the first switch valve is used to control the outflow of the mixed liquid when it is opened.

3. The system according to claim 1, characterized in that The dispersion unit includes a dispersion cup and a disperser, wherein: The dispersion cup is used to contain the sample particles and the dispersant; The disperser is used to disperse the sample particles to obtain the mixed solution.

4. The system according to claim 3, characterized in that The dispersion unit further comprises a glove box, the dispersion cup is placed inside the glove box, and the glove box is used to keep the operating environment of the dispersion cup in a closed state.

5. The system according to claim 1, characterized in that The recovery unit includes a filtering module and a storage module, wherein: The filtering module is used to filter the mixed liquid to obtain the recovered liquid of the dispersant; The storage module is used to store the recovered liquid of the dispersant.

6. The system according to claim 5, characterized in that The storage module includes a liquid storage tank and a vacuum pump, wherein: The liquid storage tank is used to store the dispersant and the recovered liquid of the dispersant, and the liquid storage tank is provided with a liquid replenishing port, and the liquid replenishing port is used to replenish the dispersant when the liquid storage capacity in the liquid storage tank is lower than a preset liquid storage capacity threshold; The vacuum pump is used to extract air from the liquid storage tank to form a vacuum environment.

7. The system according to claim 1, characterized in that The system further comprises a control unit, the delivery module comprises a peristaltic pump, and the control unit is used for controlling the delivery of a fixed amount of the dispersant by adjusting the pipeline cross-sectional area, flow rate and single delivery time of the peristaltic pump.

8. A sample particle dispersion method, characterized in that: The method comprises: Mixing sample particles and a dispersant to obtain a mixed solution of the sample particles and the dispersant; filtering the mixed solution to obtain a recovery solution of the dispersant; The recovered liquid of the dispersant is used to prepare the mixed liquid.

9. A laser particle size analyzer device, characterized in that: The laser particle size analyzer device comprises a laser particle size analyzer and the sample particle dispersion system according to any one of claims 1 to 7, wherein the laser particle size analyzer is used to detect a mixed solution of the sample particles and a dispersant.

10. The laser particle size analyzer device according to claim 9, characterized in that: The sample particles are polyolefin catalysts.

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