CN110658036A - Preparation of UHMWPE dilute solution and method for detecting dissolution degree of UHMWPE dilute solution - Google Patents
Preparation of UHMWPE dilute solution and method for detecting dissolution degree of UHMWPE dilute solution Download PDFInfo
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01N1/38—Diluting, dispersing or mixing samples
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Abstract
The invention relates to a method for preparing UHMWPE dilute solution and detecting the dissolution degree thereof, which comprises weighing dried UHMWPE powder or fine fragments with mass m1Mixing UHMWPE with a solvent, standing the mixed solution at a high temperature and a constant temperature for a period of time, and then mechanically stirring until the stirring torque is stable; filtering the mixed solution by a filter screen, collecting UHMWPE gel particles on the filter screen, extracting the UHMWPE gel particles by an extraction solvent, and drying in vacuum to obtain a mass m2In m is2/m1The value of (b) was used as a parameter for judging the dissolution degree of UHMWPE. Compared with the prior art, the invention uses m2/m1The ratio of the molecular weight and the molecular weight of the UHMWPE is used as the physical gel content to quantitatively evaluate the dissolution degree of the UHMWPE, and has important guiding significance for processing UHMWPE fibers and diaphragms.
Description
Technical Field
The invention relates to the field of organic chemical materials, in particular to a preparation method of UHMWPE dilute solution and a method for detecting the dissolution degree of the UHMWPE dilute solution.
Background
In recent years, ultrahigh molecular weight polyethylene (UHMWPE) resin and small molecular solvent are widely used in the field of high strength fibers and lithium battery separators, and due to the tightly entangled structure of UHMWPE macromolecular chains, dissolution is very difficult, and if UHMWPE resin is not completely dissolved in a solvent, transparent "gel" particles (different from gel formed by a crosslinked network, due to the fact that physical entanglement points between molecular chains are not completely disentangled in the solvent) appear in the solution, which is particularly reflected in that defects such as black spots, crystal spots or broken holes appear on the surface of a fiber or a film prepared from UHMWPE resin, and the performance and quality of a product are greatly affected, and in addition, the gel particles contained in the solution affect the processing stability of the product. Therefore, the preparation of the uniform UHMWPE solution becomes an important link in the whole production process of the fiber and the diaphragm, so that the molecular chain of the UHMWPE is fully unwound in the solvent to form the uniform solution, which has decisive influence on the performance of the fiber or the diaphragm.
The preparation of a homogeneous dilute UHMWPE solution and the detection of its degree of dissolution are critical for the processing and product performance.
Patent CN 109721892A discloses a vinylidene fluoride thermoplastic resin, a preparation method and application thereof, wherein a method for testing the gel content of a polymer is disclosed as follows: the number of defects visible to the naked eye after extrusion of the polymer into a film can be determined. The film is transparent or opaque and the defects reflect or refract light and appear as (more) opaque regions (typically shown as dark or black regions or spots). Record per m by imaging software2Such number of spots of the film gives the gel content of the polymer. The size of the defect is about 0.06mm to 1.00 mm. The method has high requirements on test samples, can form films and has certain requirements on light transmittance. In addition, the method can only measure the gel particles on the surface of the membrane, and has certain deviation from the real result.
Patent CN 109153809 a discloses a molecular modification method of polyethylene resin, which relates to a method for calculating gel content of crosslinked polyethylene by dry weighing after extracting crosslinked polyethylene with boiling xylene by a soxhlet extraction device, and the method is refluxed at high temperature for a long time to achieve complete dissolution of non-crosslinked polyethylene part, but the method is not suitable for the insoluble 'gel' particles formed by physical entanglement of macromolecular chains, because the 'gel' formed by physical entanglement points is completely dissolved in a solvent only after a sufficient period of high-temperature reflux.
Patent CN102605440A discloses a method for preparing a high-concentration ultrahigh molecular weight polyethylene spinning solution, which comprises adding ultrahigh molecular weight polyethylene powder with a molecular weight of 500 to 800 ten thousand and an antioxidant into a solvent together, and dissolving at high temperature to prepare a low-concentration ultrahigh molecular weight polyethylene solution; the high-temperature solution of the low-concentration ultrahigh molecular weight polyethylene is concentrated at 190-220 ℃ to obtain a uniform and completely dissolved 10-20% high-concentration ultrahigh molecular weight polyethylene solution, a quantitative dissolution degree measuring method is not disclosed, and the dissolution condition of the ultrahigh molecular weight polyethylene cannot be clearly determined.
Disclosure of Invention
The invention aims to solve the problems, provides a method for preparing diluted UHMWPE solution and detecting the dissolution degree of the diluted UHMWPE solution, and solves the current situation that no method for measuring the content of insoluble gel formed by physical entanglement points of macromolecular chains exists at present.
The purpose of the invention is realized by the following technical scheme:
a method for preparing diluted UHMWPE solution and detecting its solubility includes such steps as weighing dried UHMWPE powder or fine particles (mass m)1Mixing UHMWPE with a solvent, standing the mixed solution at a high temperature and a constant temperature for a period of time, and mechanically stirring until the stirring torque is stable (the torque value fluctuates within +/-5% along with the change of time within 10min to reach a stable state); then quickly filtering the mixed solution by a filter screen, collecting UHMWPE gel particles on the filter screen, extracting the UHMWPE gel particles by an extraction solvent, and drying in vacuum to obtain a mass m2In m is2/m1As a parameter for determining the degree of dissolution of UHMWPE, m2/m1The smaller the value, the degree of dissolution is indicatedThe better; on the contrary, m2/m1The larger the number, the worse the degree of dissolution. The experimental results show that m2/m1The numerical value is 0-0.5%, which shows that the dissolution degree of UHMWPE is good, and the content of gel particles is low and the particle size is small, so that the performance and appearance of the product are hardly influenced.
Preferably, the solvent is selected from one or more of decalin, paraffin oil, toluene, xylene or trichlorobenzene.
Preferably, the solvent contains an antioxidant, the antioxidant is selected from one or more of a phenolic antioxidant, an amine antioxidant and a heterocyclic antioxidant, and the concentration of the antioxidant is 0-1 wt.%.
Preferably, the gel particles are obtained by solvent extraction and drying, the extracting agent is selected from one of dichloromethane or hydrocarbon extracting agents, the extraction ratio is 50, and the vacuum drying temperature is 60-80 ℃.
Preferably, the viscosity average molecular weight of the UHMWPE resin is in the range of 0.5 x 106～5.8×106g/mol, concentration range of 0.05-0.5 wt.%.
Preferably, the temperature range of the mixed solution at the high temperature and the constant temperature is 130-200 ℃, the standing time is 0.5-3 h, further preferably 150-170 ℃, the standing time is 1-2 h, the solubility of the organic solvent to UHMWP is higher in the temperature range, and UHMWPE particles cannot exist in the formed UHMWPE dilute solution due to saturation; too long a standing time will result in the formation of a "gel" of physical entanglement which will eventually dissolve completely in the solvent.
Preferably, the rotation speed of the mechanical stirring is 100-200 rpm.
Preferably, the mesh number of the filter screen is 180-220 meshes, the mesh number of the filter screen is selected according to the molecular size of UHMWPE, and other impurities which are not in the particle size range are prevented from being filtered.
Preferably, the filter screen is a metal filter screen, and during filtering, the metal filter screen is soaked in the UHMWPE dilute solution subjected to high-temperature constant-temperature bath, and after standing for a period of time, UHMWPE gel particles on the filter screen are filtered and collected.
Preferably, the filtering time is 20-30 s, and the filtering is completed quickly. When the filter screen is used for filtering operation, the filter screen is taken out of the dilute solution, the temperature of the filter screen is reduced, the dilute solution attached to the surface of the filter screen is also cooled, the UHMWPE part can be separated out, the rapid filtering can reduce the occurrence of the conditions, and the influence on the evaluation result is reduced.
The invention is different from the existing patent for testing the gel content of the polymer formed by a chemical crosslinking network, and creatively combines m2/m1The value of (A) is (the mass of UHMWPE gel particles)/(the mass of UHMWPE resin powder)) is used as the ratio of the parameters for judging the dissolution degree of UHMWPE, the physical gel content is used for quantitatively evaluating the dissolution degree of UHMWPE, and the smaller the numerical value is, the better the dissolution degree of the UHMWPE in a solvent is, and the value has important guiding significance for processing UHMWPE fibers and diaphragms. The polymer with a cross-linked structure can not be dissolved in the solvent at the elevated temperature or for a prolonged dissolution time, and the 'gel' particles in the patent are formed by the physical entanglement points among macromolecular chains which can not be completely disentangled in the solvent, can not be dissolved in the solvent in a short time, and can be fully dissolved in the solvent at the elevated temperature or for the prolonged dissolution time. For practical production, too long a dissolution time affects the production efficiency, and an increase in temperature causes decomposition of the polymer, so that the content of "gel" particles that are not completely dissolved in the ultra-high molecular weight polyethylene resin is minimized in the processing time so as not to affect the properties of the product.
Compared with the prior art, the method adopted by the patent is different from the existing method for detecting and judging the processability (dissolution degree) of the ultra-high molecular weight polyethylene by the flaws such as transparent spots of produced products, and the method used by the patent firstly provides the characteristic that the solubility of the ultra-high molecular weight polyethylene resin can be quantitatively represented in the raw material proportioning stage, thus being beneficial to accurately screening raw materials and improving the yield of industrial production.
Compared with the prior art, the dilute UHMWPE solution prepared by the method has uniform concentration, simple preparation method and process, simple and efficient detection method, and accurate detection standard to reflect the content of the gel particles of the UHMWPE resin which are not easy to dissolve due to physical entanglement of macromolecular chains.
Detailed Description
The present invention will be described in detail with reference to specific examples.
A preparation method of diluted solution of ultra-high molecular weight polyethylene (UHMWPE) specifically comprises the following steps: respectively weighing UHMWPE resin powder, an organic solvent and an antioxidant, adding the UHMWPE resin powder, the organic solvent and the antioxidant into a container, mixing to form a dilute solution, placing the container filled with the dilute solution in a high-temperature constant-temperature bath for standing, and stirring for auxiliary dissolution to form a uniform UHMWPE dilute solution, wherein the temperature range of the high-temperature constant-temperature bath is 130-200 ℃, and the standing time is 0.5-3 h. The stirring time is 0.5-3 h. The method for detecting the dissolution degree specifically comprises the following steps: soaking a metal filter screen in dilute UHMWPE solution subjected to high-temperature constant-temperature bath, standing for a period of time, filtering and collecting UHMWPE gel particles on the filter screen, extracting and filtering the UHMWPE gel particles, weighing, and using the ratio of (the mass of the UHMWPE gel particles)/(the mass of the UHMWPE resin powder) to evaluate the dissolution degree of UHMWPE, wherein the smaller the ratio is, the higher the dissolution degree is. The mesh range of the metal filter screen is 180-220 meshes, and the filtering time is 20-30 s.
Example 1
Weighing UHMWPE (viscosity average molecular weight of 0.5 multiplied by 10)6g/mol) resin powder 0.025g, weighing 49.95g of paraffin oil, adding antioxidant 168 (the concentration is 1 wt.%), adding UHMWPE powder, paraffin oil and antioxidant into a glass container to form a dilute solution (the concentration of UHMWPE is 0.05 wt.%), placing the mixed solution of UHMWPE and paraffin oil in a constant-temperature bath at 150 ℃ for standing for 1h, and then slowly and mechanically stirring for assisting dissolution for 2h until no obvious large fluctuation appears on a torque curve along with time, which indicates that UHMWPE is dissolved to form a uniform dilute solution. Then the homogeneous solution is rapidly (within 30 s) filtered through a 200-mesh metal net to filter the high-temperature UHMWPE solution (150 ℃), UHMWPE gel particles on the filter net are collected, the solvent in the UHMWPE gel particles is extracted and dried, then the mass of the gel particles is weighed to be 0g, and the content of physical gel particles is 0%.
Example 2
Weighing UHMWPE (viscosity average molecular weight is 1.2 multiplied by 10)6g/mol) resin powder 0.05g, weighing 49.95g decalin, adding antioxidant 168 (the concentration is 1 wt.%), adding UHMWPE powder, decalin and antioxidant into a glass container to form a dilute solution (the concentration of UHMWPE is 0.1 wt.%), placing the mixed solution of UHMWPE/decalin in a constant-temperature bath at 150 ℃ for standing for 1h, then adding mechanical stirring for assisting dissolution for 1.5h until the torque is stable, and uniformly dissolving UHMWPE in a solvent by visual inspection to form a uniform solution. Then the homogeneous solution is rapidly (within 30 s) filtered through a 200-mesh metal net to filter the high-temperature UHMWPE solution (150 ℃), UHMWPE gel particles on the filter net are collected, the solvent in the UHMWPE gel particles is extracted and dried, then the mass of the gel particles is weighed to be 0g, and the content of physical gel particles is 0%.
Example 3
Weighing UHMWPE (viscosity average molecular weight is 2.1 multiplied by 10)6g/mol) resin powder 0.25g, weighing 49.75g paraffin oil, adding antioxidant 168 (the concentration is 0.5 wt.%), adding UHMWPE powder, paraffin oil and antioxidant into a glass container to form a dilute solution (the concentration of UHMWPE is 0.5 wt.%), placing the mixed solution of UHMWPE/decalin in a constant-temperature bath at 160 ℃ for standing for 1h, then adding mechanical stirring for assisting dissolution for 1.5h until the torque is stable, and visually observing that UHMWPE is uniformly dissolved in a solvent to form a uniform solution. Then the homogeneous solution is rapidly (within 30 s) filtered through a 200-mesh metal net to filter the high-temperature UHMWPE solution (160 ℃), UHMWPE gel particles on the filter screen are collected, the solvent in the UHMWPE gel particles is extracted and dried, and then the mass of the gel particles is weighed to be 0.008g, so that the content of physical 'gel' particles is 3.2%.
Example 4
Weighing UHMWPE (viscosity average molecular weight is 3.5 multiplied by 10)6g/mol) resin powder 0.25g, weighing 49.75g decalin, adding antioxidant 168 (the concentration is 0.6 wt.%), adding UHMWPE powder, decalin and antioxidant into a glass container to form a dilute solution (the concentration of UHMWPE is 0.5 wt.%), placing the mixed solution of UHMWPE/decalin in a constant-temperature bath at 150 ℃ for standing for 1h, then adding mechanical stirring for assisting dissolution for 1.5h until the torque is stable, and visually observing that UHMWPE is uniformly dissolved in a solvent to form a uniform solution.Then the homogeneous solution is rapidly (within 30 s) filtered through a 200-mesh metal net to filter the high-temperature UHMWPE solution (150 ℃), UHMWPE gel particles on the filter net are collected, the solvent in the UHMWPE gel particles is extracted and dried, and then the mass of the gel particles is weighed to be 0.015g, so that the content of physical gel particles is 6%.
Example 5
Weighing UHMWPE (viscosity average molecular weight is 5.8 multiplied by 10)6g/mol) resin powder 0.25g, weighing 49.75g paraffin oil, adding antioxidant 168 (the concentration is 1 wt.%), adding UHMWPE powder, paraffin oil and antioxidant into a glass container to form a dilute solution (the concentration of UHMWPE is 0.5 wt.%), placing the mixed solution of UHMWPE/decalin in a constant-temperature bath at 180 ℃ for standing for 1h, then adding mechanical stirring for assisting dissolution for 2h until the torque is stable, and visually observing that the UHMWPE is uniformly dissolved in the solvent to form a uniform solution. Then the homogeneous solution is rapidly (within 30 s) filtered through a 200-mesh metal net to filter the high-temperature UHMWPE solution (180 ℃), UHMWPE gel particles on the filter screen are collected, the solvent in the UHMWPE gel particles is extracted and dried, the mass of the gel particles is weighed to be 0.021g, and then the content of physical gel particles is 8.4%.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A method for preparing diluted UHMWPE solution and detecting its dissolving degree is characterized by that said method includes weighing dried UHMWPE powder or fine fragment whose mass is m1Mixing UHMWPE with a solvent, standing the mixed solution at a high temperature and a constant temperature for a period of time, and then mechanically stirring until the stirring torque is stable; then quickly filtering the mixed solution by a filter screen, collecting UHMWPE gel particles on the filter screen, and extracting the gel particles by an extraction solventMass after vacuum drying is m2In m is2/m1The value of (b) was used as a parameter for judging the dissolution degree of UHMWPE.
2. The method for preparing the dilute UHMWPE solution and detecting the dissolution degree thereof according to claim 1, characterized in that the solvent is one or more selected from decalin, paraffin oil, toluene, xylene or trichlorobenzene.
3. The method for preparing the dilute UHMWPE solution and detecting the dissolution degree of the dilute UHMWPE solution as claimed in claim 2, wherein the solvent contains an antioxidant, the antioxidant is selected from one or more of a phenolic antioxidant, an amine antioxidant and a heterocyclic antioxidant, and the concentration of the antioxidant is 0-1 wt.%.
4. The method for preparing the dilute UHMWPE solution and detecting the dissolution degree thereof according to claim 1, characterized in that the gel particles are obtained by extracting and drying with a solvent, the extracting agent is one of dichloromethane or hydrocarbon extracting agent, the extraction ratio is 50, and the temperature for vacuum drying is 60-80 ℃.
5. The method for preparing diluted UHMWPE solution and detecting its dissolution degree according to claim 1, characterized in that the viscosity average molecular weight of UHMWPE resin is in the range of 0.5 x 106～5.8×106g/mol, concentration range of 0.05-0.5 wt.%.
6. The method for preparing the dilute UHMWPE solution and detecting the dissolution degree of the dilute UHMWPE solution as claimed in claim 1, wherein the temperature range of the mixed solution at the high temperature and the constant temperature is 130-200 ℃, and the standing time is 0.5-3 h.
7. The method for preparing diluted UHMWPE solution and detecting its dissolution degree according to claim 1, characterized in that the rotation speed of the mechanical stirring is in the range of 100rpm to 200 rpm.
8. The method for preparing dilute UHMWPE solution and detecting its dissolution degree according to claim 1, characterized in that the torque value fluctuates within ± 5% with time within 10min to reach a steady state.
9. The method for preparing the dilute UHMWPE solution and detecting the dissolution degree of the dilute UHMWPE solution as claimed in claim 1, wherein the filter screen is a metal filter screen, during the filtration, the metal filter screen is soaked in the dilute UHMWPE solution which is subjected to a high-temperature constant-temperature bath, after standing for a period of time, UHMWPE gel particles on the filter screen are rapidly filtered and collected, and the mesh number of the filter screen is 180-220 meshes.
10. The method for preparing the dilute UHMWPE solution and detecting the dissolution degree thereof according to claim 9, characterized in that the filtration time is 20-30 s.
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