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Method for preparing dilute UHMWPE solution and detecting its dissolution degree

A dilute solution and degree technology, which is applied in the preparation of UHMWPE dilute solution and the detection of its solubility, can solve the problem of not measuring the "gel" content, and achieve the effect of simple detection method, improved yield and efficient detection standard.

Active Publication Date: 2020-01-07
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a method for the preparation of UHMWPE dilute solution and its dissolution degree detection in order to solve the above problems, and solve the problem of not measuring the content of the insoluble "gel" formed by the physical entanglement points of macromolecular chains at present. The current state of the method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh UHMWPE (viscosity average molecular weight is 0.5 × 10 6 g / mol) resin powder 0.025g, weigh 49.95g paraffin oil, add antioxidant 168 (concentration is 1wt.%), UHMWPE powder, paraffin oil, antioxidant are added in the glass container, form dilute solution (UHMWPE concentration is 0.05wt.%), the UHMWPE / paraffin oil mixture was placed in a constant temperature bath at 150°C for 1 hour, and then slowly mechanically stirred to assist dissolution for 2 hours, until the curve of torque versus time did not show significant fluctuations, indicating that the UHMWPE was dissolved A homogeneous dilute solution was formed. Then quickly (within 30s) filter the high-temperature UHMWPE solution (150°C) through a 200-mesh metal mesh, collect the UHMWPE gel particles on the filter, extract and dry the solvent, and weigh the mass of the gel particles to 0g , then the content of physical "gel" particles is 0%.

Embodiment 2

[0027] Weigh UHMWPE (viscosity average molecular weight is 1.2 * 10 6g / mol) resin powder 0.05g, weigh 49.95g decahydronaphthalene, add antioxidant 168 (concentration is 1wt.%), UHMWPE powder, decahydronaphthalene, antioxidant are added in the glass container, form dilute solution (UHMWPE The concentration is 0.1wt.%), put the mixture of UHMWPE / decalin in a 150°C constant temperature bath and let it stand for 1h, and then dissolve it with mechanical stirring for 1.5h, until the torque is stable, and the UHMWPE is uniformly dissolved in the solvent to form homogeneous solution. Then quickly (within 30s) filter the high-temperature UHMWPE solution (150°C) through a 200-mesh metal mesh, collect the UHMWPE gel particles on the filter, extract and dry the solvent, and then weigh the mass of the gel particles. g, then the content of physical "gel" particles is 0%.

Embodiment 3

[0029] Weigh UHMWPE (viscosity-average molecular weight is 2.1 × 10 6 g / mol) resin powder 0.25g, weigh 49.75g paraffin oil, add antioxidant 168 (concentration is 0.5wt.%), UHMWPE powder, paraffin oil, antioxidant are added in the glass container, form dilute solution (UHMWPE concentration 0.5wt.%), the UHMWPE / decalin mixture was placed in a constant temperature bath at 160°C for 1 hour, and then assisted by mechanical stirring for 1.5 hours until the torque was stable, and the UHMWPE was uniformly dissolved in the solvent to form a uniform solution. Then quickly (within 30s) pass the uniform solution through a 200-mesh metal mesh to filter the high-temperature UHMWPE solution (160°C), collect the UHMWPE gel particles on the filter, extract and dry the solvent, and weigh the gel particle mass to 0.008 g, then the content of physical "gel" particles is 3.2%.

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Abstract

The invention relates to a method for preparing a dilute UHMWPE solution and detecting its dissolution degree, and the method comprises the following steps of weighing dry UHMWPE powder or fine fragments with the mass meter of m1, mixing UHMWPE with a solvent, performing mechanical stirring after placing the mixed solution at a high temperature and constant temperature for a period of time until the stirring torque is stable; filtering the mixed liquid through a filter screen, collecting UHMWPE gel particles on the filter screen, defining the mass meter after vacuum drying as m2 through the solvent extraction, and taking the value of m2 / m1 as a parameter to judge the degree of UHMWPE dissolution. Compared with the prior art, the invention uses the m2 / m1 ratio as the physical "gel" contentfor quantitatively evaluating the degree of UHMWPE dissolution, and has important guiding significance for the processing of UHMWPE fibers and separators.

Description

technical field [0001] The invention relates to the field of organic chemical materials, in particular to a method for preparing UHMWPE dilute solution and detecting its dissolution degree. Background technique [0002] In recent years, the processing of ultra-high molecular weight polyethylene (UHMWPE) resin and small molecule solvents has been widely used in the fields of high-strength fibers and lithium battery separators. Due to the tightly entangled structure of UHMWPE macromolecular chains, it is very difficult to dissolve it. If UHMWPE If the resin is not completely dissolved in the solvent, transparent "gel" particles will appear in the solution (formed because the physical entanglement points between molecular chains cannot be completely disentangled in the solvent, which is different from the gel formed by the cross-linked network. ), specifically manifested in the appearance of black spots, crystal points or holes on the surface of the fiber or film prepared by UH...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N1/38G01N5/04
CPCG01N1/286G01N1/38G01N5/04
Inventor 茆汉军徐迅张文阳张玉梅王新威孙勇飞
Owner SHANGHAI RES INST OF CHEM IND
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