CN112730174A - Method for monitoring concentration of spheroidal particles in crystallization process in real time - Google Patents
Method for monitoring concentration of spheroidal particles in crystallization process in real time Download PDFInfo
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- CN112730174A CN112730174A CN202011491578.3A CN202011491578A CN112730174A CN 112730174 A CN112730174 A CN 112730174A CN 202011491578 A CN202011491578 A CN 202011491578A CN 112730174 A CN112730174 A CN 112730174A
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- spheroidal particles
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- 239000002245 particle Substances 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 53
- 238000002425 crystallisation Methods 0.000 title claims abstract description 27
- 230000008025 crystallization Effects 0.000 title claims abstract description 27
- 238000012544 monitoring process Methods 0.000 title claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 20
- 238000012634 optical imaging Methods 0.000 claims abstract description 12
- 238000012545 processing Methods 0.000 claims abstract description 11
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 239000004677 Nylon Substances 0.000 claims description 15
- 229920001778 nylon Polymers 0.000 claims description 15
- 238000002834 transmittance Methods 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 2
- -1 polypropylene Polymers 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- 239000012798 spherical particle Substances 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 10
- 230000002776 aggregation Effects 0.000 abstract description 3
- 238000004220 aggregation Methods 0.000 abstract description 3
- 238000005070 sampling Methods 0.000 description 8
- 238000005259 measurement Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 230000005514 two-phase flow Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/06—Investigating concentration of particle suspensions
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- G01N15/075—
Abstract
The invention discloses a method for monitoring the concentration of spheroidal particles in a crystallization process in real time, which comprises the following steps: 1) preparing a series of spheroidal particle suspensions with different concentrations; 2) observing and intercepting the suspension liquid in a stirring state by using a two-dimensional optical imaging system, and processing the intercepted image into a two-dimensional image; 3) calculating the total number of pixels of the spheroidal particles in the two-dimensional image, and establishing a concentration-total number of pixels standard curve; 4) and (3) carrying out real-time observation and image interception on the reaction liquid in the crystallization process by using a two-dimensional optical imaging system, processing the intercepted image into a two-dimensional image, then calculating the total number of pixels of the spheroidal particles, and obtaining real-time concentration data of the spheroidal particles according to the concentration-total number of pixels standard curve in the step 3). The method can monitor the concentration of the spheroidal particles in the crystallization process in real time, has higher accuracy, and can obtain crystal aggregation information according to the real-time change condition of the concentration.
Description
Technical Field
The invention relates to the technical field of concentration measurement, in particular to a method for monitoring the concentration of spheroidal particles in a crystallization process in real time.
Background
The particle concentration measurement in the material crystallization process, especially the real-time measurement of the concentration of the spheroidal crystal particles, has very important significance for researching the crystal nucleation process and the crystal growth process. At present, the methods for measuring the concentration of solid particles in two-phase flow mainly include the following methods: 1) the off-line sampling analysis method has the disadvantages that the operation of the method is very complicated, the concentration of samples obtained from different positions is greatly different, and the sampling operation can cause the reaction system to change to influence the crystallization process; 2) the screening method mainly obtains the concentration information of crystal particles after crystallization is finished, and the concentration of the particles in the crystallization process cannot be monitored in real time; 3) the concentration of solid particles in the solution is measured by a focused beam reflectivity measuring technology, the method has the problem that information obtained by measuring the focused beam reflectivity cannot reflect the influence caused by crystal aggregation, and the accuracy of a test result is low.
Therefore, there is a need to develop a method that can monitor the concentration of spheroidal particles in the crystallization process in real time.
Disclosure of Invention
The invention aims to provide a method for monitoring the concentration of spheroidal particles in a crystallization process in real time.
The technical scheme adopted by the invention is as follows:
a method for monitoring the concentration of spheroidal particles in a crystallization process in real time comprises the following steps:
1) preparing a series of spheroidal particle suspensions with different concentrations;
2) observing and intercepting the suspension liquid in a stirring state by using a two-dimensional optical imaging system, and processing the intercepted image into a two-dimensional image;
3) calculating the total number of pixels of the spheroidal particles in the two-dimensional image, and establishing a concentration-total number of pixels standard curve;
4) and (3) carrying out real-time observation and image interception on the reaction liquid in the crystallization process by using a two-dimensional optical imaging system, processing the intercepted image into a two-dimensional image, then calculating the total number of pixels of the spheroidal particles, and obtaining real-time concentration data of the spheroidal particles according to the concentration-total number of pixels standard curve in the step 3).
Preferably, the method for monitoring the concentration of the spheroidal particles in the crystallization process in real time comprises the following steps:
1) respectively preparing 1%, 2%, 3%, 4%, 5%, 7%, 10% and 12% of spheroidal particle suspension by mass fraction;
2) observing and intercepting the suspension liquid in a stirring state by using a two-dimensional optical imaging system, and processing the intercepted image into a two-dimensional image;
3) calculating the total number of pixels of the spheroidal particles in the two-dimensional image, and establishing a concentration-total number of pixels standard curve;
4) and (3) carrying out real-time observation and image interception on the reaction liquid in the crystallization process by using a two-dimensional optical imaging system, processing the intercepted image into a two-dimensional image, then calculating the total number of pixels of the spheroidal particles, and obtaining real-time concentration data of the spheroidal particles according to the concentration-total number of pixels standard curve in the step 3).
Preferably, the particle size of the spheroidal particles in the step 1) is 50-125 μm.
Preferably, the mass fraction of the spheroidal particle suspension in the step 1) is 1-15%.
Preferably, the light transmittance of the suspension of spheroidal particles in step 1) is greater than 60%.
Preferably, the spheroidal particles in step 1) are one of nylon particles and polypropylene particles.
The invention has the beneficial effects that: the method can monitor the concentration of the spheroidal particles (the spheroidal particles cannot generate measurement errors due to shooting angles, and the measurement errors caused by small density differences of different crystal forms of the spheroidal crystal particles in the growth process) in real time in the crystallization process, has high accuracy, can obtain crystal aggregation information according to the real-time change condition of the concentration, and has very important significance for researching the crystal nucleation and growth processes.
Drawings
Fig. 1 is a perspective view of a suspension of 3% by mass of nylon particles in example 1.
Fig. 2 is a two-dimensional image of a suspension of 3% by mass of nylon particles in example 1.
FIG. 3 is a standard curve of concentration versus total number of pixels in example 1.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
Example 1:
a method for monitoring the particle concentration of nylon resin in a cooling crystallization process in real time comprises the following steps:
1) dispersing nylon particles in water, and respectively preparing nylon particle (particle size is 50-125 microns) suspensions (light transmittance is more than 60%) with the mass fractions of 1%, 2%, 3%, 4%, 5%, 7%, 10% and 12%;
2) observing and image-intercepting the suspension in a stirring state by using a two-dimensional optical imaging system (CN 205280541U probe type process imager), and processing the intercepted image into a two-dimensional image (a three-dimensional image of the nylon particle suspension with the mass fraction of 3% is shown in figure 1, and a two-dimensional image of the nylon particle suspension with the mass fraction of 3% is shown in figure 2);
3) calculating the total number of pixels of the nylon particles in the two-dimensional image, and establishing a concentration-total number of pixels standard curve (shown in figure 3);
4) cooling and crystallizing the nylon resin, wherein the crystallizing operation lasts for 3 hours totally, a two-dimensional optical imaging system (CN 205280541U probe type process imager) is used for carrying out real-time observation and image interception on the reaction liquid once per second, the intercepted image is processed into a two-dimensional image, then the total number of pixels of the nylon particles is calculated, calculating and outputting nylon particle concentration data according to the concentration-pixel total number standard curve obtained in the step 3), simultaneously performing off-line sampling test, recording the time point of off-line measurement sampling, calculating the average nylon particle concentration within 1min before and after the off-line measurement sampling time point obtained by the method of the invention, which is 1.06 wt%, 2.10 wt%, 3.46 wt%, 4.84 wt% and 5.89 wt% in sequence, while the concentrations of nylon particles measured using the off-line sampling method were 1.26 wt%, 2.49 wt%, 3.69 wt%, 4.86 wt%, and 6.00 wt%.
From example 1, it can be seen that: the method provided by the invention is simple to operate, the obtained test result is high in accuracy, the change condition of the particle concentration in the solution can be monitored in real time, the problem that the concentration of samples obtained from different positions is greatly different and the problem that the crystallization process is influenced due to the change of a reaction system caused by the sampling operation easily occurring in the offline sampling method is solved.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (6)
1. A method for monitoring the concentration of spheroidal particles in a crystallization process in real time is characterized by comprising the following steps:
1) preparing a series of spheroidal particle suspensions with different concentrations;
2) observing and intercepting the suspension liquid in a stirring state by using a two-dimensional optical imaging system, and processing the intercepted image into a two-dimensional image;
3) calculating the total number of pixels of the spheroidal particles in the two-dimensional image, and establishing a concentration-total number of pixels standard curve;
4) and (3) carrying out real-time observation and image interception on the reaction liquid in the crystallization process by using a two-dimensional optical imaging system, processing the intercepted image into a two-dimensional image, then calculating the total number of pixels of the spheroidal particles, and obtaining real-time concentration data of the spheroidal particles according to the concentration-total number of pixels standard curve in the step 3).
2. The method of real-time monitoring of concentration of spheroidal particles during crystallization according to claim 1, comprising the steps of:
1) respectively preparing 1%, 2%, 3%, 4%, 5%, 7%, 10% and 12% of spheroidal particle suspension by mass fraction;
2) observing and intercepting the suspension liquid in a stirring state by using a two-dimensional optical imaging system, and processing the intercepted image into a two-dimensional image;
3) calculating the total number of pixels of the spheroidal particles in the two-dimensional image, and establishing a concentration-total number of pixels standard curve;
4) and (3) carrying out real-time observation and image interception on the reaction liquid in the crystallization process by using a two-dimensional optical imaging system, processing the intercepted image into a two-dimensional image, then calculating the total number of pixels of the spheroidal particles, and obtaining real-time concentration data of the spheroidal particles according to the concentration-total number of pixels standard curve in the step 3).
3. The method of real-time monitoring of concentration of spheroidal particles during crystallization according to claim 1 or 2, wherein: the particle diameter of the spheroidal particles in the step 1) is 50-125 μm.
4. The method of real-time monitoring of concentration of spheroidal particles during crystallization according to claim 1 or 2, wherein: the mass fraction of the quasi-spherical particle suspension in the step 1) is 1-12%.
5. The method of real-time monitoring of concentration of spheroidal particles during crystallization according to claim 1 or 2, wherein: the light transmittance of the spheroidal particle suspension of step 1) is greater than 60%.
6. The method of real-time monitoring of concentration of spheroidal particles during crystallization according to claim 1 or 2, wherein: the sphere-like particles in the step 1) are one of nylon particles and polypropylene particles.
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Application publication date: 20210430 |