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Method for detecting gel particles in PAN spinning solution

A spinning dope and detection method technology, applied in the field of PAN wet spinning, can solve the problems of error in measurement results, time-consuming, inability to quantitatively express the size and number of gel particles, etc., and achieves short operation time and operation. Simple, improved spinning stability

Pending Publication Date: 2021-12-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Report on the characterization method of gel particles: dynamic light scattering method, by observing the distribution of scattered light intensity corresponding to different gelation stages, to judge whether the system undergoes gelation transition, at a certain time during the test, the scattered light The intensity shows a strong fluctuation, observe the time point when the gel appears, but this method cannot quantitatively express the particle size and particle number of the gel; the brightness value measurement method is to measure the color difference brightness value during the gel formation process of the system The dynamic change is used to characterize the gel point. This method shows the dynamic change of the gel formation of the system well, and the gel process is divided into three stages: sol, sol-gel transition region, and complete gel region, but also The gel particles are not quantitatively characterized; the rheological method is a powerful tool to study the gelation behavior of polymer solutions, and the different variables of gelation can be determined, which can be divided into temperature gel point, concentration gel point, time gel Points, etc., this method cannot calibrate the size of the gel particles; the method of filtration measures the content of the gel particles of the PAN stock solution, this method requires a large amount of stock solution, takes a long time and is difficult to quantitatively measure, the gel particles are in the process of filtration , will be deformed under the influence of pressure rise, so that it will pass through the filter, causing errors in the measurement results; the method of centrifugal separation, this method is only applicable to PAN stock solution with more particles and larger particle size

Method used

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  • Method for detecting gel particles in PAN spinning solution
  • Method for detecting gel particles in PAN spinning solution
  • Method for detecting gel particles in PAN spinning solution

Examples

Experimental program
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Effect test

Embodiment 1

[0034] A kind of detection method of gel particle in PAN spinning dope, concrete steps are as follows:

[0035] (1) PAN spinning stock solution I whose solvent is NaSCN solution, filter out the impurities in the stock solution through a filter cloth with a pore size of 100 μm, then stand at 25°C for 8 hours, and then defoam in a vacuum oven at a temperature of 35°C After 6 hours, the spinning stock solution II was obtained; using the method of heterogeneous film formation, the spinning stock solution II was poured on a glass plate with a flat and smooth surface and a bacterial cellulose film, and the AFA-II automatic film applicator was used to spread it evenly into 100 μm thickness, then put the prepared film into a tray filled with distilled water for 30 minutes, and finally rinse repeatedly to remove the solvent in the film, and air dry naturally to obtain a PAN film;

[0036] The solid content of PAN in the above-mentioned spinning dope II is 5%, the weight average molecul...

Embodiment 2

[0047] A kind of detection method of gel particle in PAN spinning dope, concrete steps are as follows:

[0048] (1) The PAN spinning stock solution I whose solvent is NaSCN solution, filter the impurities in the stock solution through a filter cloth with a pore size of 100 μm, then stand at 26°C for defoaming for 10 hours, and then defoam in a vacuum oven at a temperature of 37°C After 5 hours, the spinning stock solution II was obtained; using the method of heterogeneous film formation, the spinning stock solution II was poured on a glass plate with a smooth surface and a bacterial cellulose film, and the AFA-II automatic film applicator was used to spread it evenly into 100 μm thickness, then put the prepared film into a tray filled with distilled water for 30 minutes, and finally rinse repeatedly to remove the solvent in the film, and dry naturally to obtain a PAN film containing gel particles;

[0049] The solid content of PAN in the above-mentioned spinning dope II is 10%...

Embodiment 3

[0060] A method for detecting particles in a PAN spinning stock solution gel, the specific steps are as follows:

[0061] (1) The PAN spinning stock solution I whose solvent is NaSCN solution, filter the impurities in the stock solution through a filter cloth with a pore size of 100 μm, then stand at 27°C for 9 hours, and then defoam in a vacuum oven at a temperature of 39°C After 4 hours, the spinning stock solution II was obtained; using the method of heterogeneous film formation, the spinning stock solution II was poured on a glass plate with a flat and smooth surface and a bacterial cellulose film, and the AFA-II automatic film applicator was used to spread it evenly into 50 μm thickness, then put the prepared film into a tray filled with distilled water for 30 minutes, and finally rinse repeatedly to remove the solvent in the film, and dry naturally to obtain a PAN film containing gel particles;

[0062] The solid content of PAN in the above-mentioned spinning dope II is ...

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Abstract

The invention relates to a method for detecting gel particles in a PAN spinning solution. The method comprises the steps of preparing a PAN film from a filtered and defoamed PAN spinning solution, dyeing the PAN film, putting the dyed PAN film under a microscope to take a picture, finally, carrying out image processing on the picture by using image processing software to read dyeing abnormal points caused by gel particles, and obtaining the number and the particle size of gel particles in the PAN spinning solution according to the dyeing abnormal points. The method can quantitatively characterize the number and the particle size of the gel particles. The method disclosed by the invention is simple to operate and short in operation time, and the morphology, size and quantity of the gel particles can be quantitatively and stereoscopically analyzed; and the spinning stability is improved, scheme and benefit prediction is carried out on spinning, and the method has great application prospects.

Description

technical field [0001] The invention belongs to the technical field of PAN wet spinning, and in particular relates to a detection method for gel particles in PAN spinning stock solution. Background technique [0002] The gel particles in the PAN spinning stock solution seriously affect the production efficiency and production continuity of acrylic fibers. It is very important to analyze the formation reasons of the gel particles and characterize the properties of the gel particles for industrial production. Now there are a lot of information about the PAN gel mechanism. reports. The literature (10.1016 / j.polymer.2008.10.013, 10.1021 / jp809701b) took the PAN stock solution with DMSO as the solvent and 15-23wt% polymer concentration as the object, and studied the factors such as polymer concentration, temperature, aging time and non-solvent The impact on the gelation behavior of PAN found that the origin of the PAN gel in this system is not the microcrystalline nucleus, but is...

Claims

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Application Information

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IPC IPC(8): G01N15/02G01N15/10G01N1/28G01N1/30G06T7/00G06T7/13G06T11/20
CPCG01N15/0205G01N15/10G01N1/2813G01N1/30G06T7/0004G06T7/13G06T11/206G06T2207/10056G06T2207/30124G06T2207/30242G01N2015/1024
Inventor 王彪李文陈忠东黄利捷吴永隽江明亮王旺祥王玉奎朱训农王伟
Owner CHINA PETROLEUM & CHEM CORP
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