CN111024749A - Method for evaluating spinning post-processing performance based on differential scanning calorimetry - Google Patents
Method for evaluating spinning post-processing performance based on differential scanning calorimetry Download PDFInfo
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Abstract
The invention relates to a method for evaluating the processability after spinning based on differential scanning calorimetry, belonging to the technical field of spinning. The invention adopts DSC (differential scanning calorimetry) analysis to test the crystallization performance of POY protofilament and the crystallization performance of dry slices, fully simulates two processes of thermal crystallization and cold crystallization of macromolecules in the false twisting process of POY, and evaluates the processability of POY through the analysis of the crystallization temperature and the crystallization rate value.
Description
Technical Field
The invention relates to a method for evaluating the processability after spinning based on differential scanning calorimetry, belonging to the technical field of spinning.
Background
Thermal analysis is an important analysis and test means in the field of use of high molecular polymer materials. DSC (differential scanning calorimetry) refers to the difference in heat between a test sample and a reference during a programmed temperature (rise/fall/constant temperature and combinations thereof) to characterize all physical and chemical changes associated with thermal effects. And can be fully applied to items such as glass transition, crystallization, melting and crystallization capability analysis, etc.
The requirements of the colored yarn for the color uniformity, the quality stability, the wear resistance and the weather resistance of the colored yarn for the vehicle are stricter than those of the common DTY yarn, so the quality index of the POY, particularly the processability of post processing (drafting false twisting), is particularly important.
In the production process of the colored yarn for the vehicle, due to the addition of the pigment powder, namely, a plurality of crystal nuclei are added into the high molecular polymer, the crystallization process is greatly influenced, and the post-processing process is greatly influenced, so that the factor must be fully considered when the quality of the POY yarn for the vehicle is evaluated.
The drying of the slices is an important technical process of polyester spinning, and the stability of the spinning and the post-processing performance of POY protofilament are directly influenced by the quality of the drying effect.
At present, POY yarn manufacturers and the current national standards test physical indexes (breaking strength, breaking elongation, evenness value and the like) and variation coefficients, and whether the physical indexes and the variation coefficients are within a certain range is judged to judge the quality of the POY; and more foreign manufacturers relatively simulate the stress test of the heated yarn in the post-processing process, and judge the quality of the POY through the absolute value and the uniformity of the stress.
Similarly, the polyester PET industry and the current national standard evaluate the drying effect by the water content of the dried slices, and the common standard is less than 30 mg/kg. In actual production, the drying temperature is 165-190 ℃, and the water content of slices does not change obviously after the drying time is 3-4 hours. However, in practice, the size and distribution of molecular weight, the difference in intrinsic viscosity, and the flow property of the polyester chips are changed with the change of time and temperature, and thus the spinning performance is substantially affected.
In view of the above-mentioned drawbacks, the present designer has made active research and innovation to create a method for evaluating the processability after spinning based on differential scanning calorimetry, so that the method has industrial utility value.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a method for evaluating the processability after spinning based on differential scanning calorimetry.
The invention adopts DSC (differential scanning calorimetry) analysis to test the crystallization performance of POY protofilament, fully simulates two processes of thermal crystallization and cold crystallization of high polymer in the false twisting process of POY, and evaluates the quality of POY, especially the quality of processability, by analyzing the numerical values of crystallization temperature and crystallization rate; the invention also adopts DSC (differential scanning calorimetry) analysis to test the crystallization performance of the dried slice, and evaluates the drying effect of the slice through the high and low crystallization temperature and the high and low crystallization rate.
The invention relates to a method for evaluating spinning post-processing performance based on differential scanning calorimetry, which combines the differential scanning calorimetry technology with the calculation of a thermal analysis dynamics theoretical formula to evaluate the spinning post-processing performance and comprises the following specific steps:
(1) cutting 8-10 mg of a sample to be evaluated into pieces, putting the pieces into a sample vessel, and putting the sample vessel into a differential scanning calorimeter;
(2) performing DSC measurement by using a differential scanning calorimeter, introducing nitrogen at a flow rate of 20ml/min for protection, setting a heating rate of 10 ℃/min, heating to 290 ℃, and keeping for 5 min; then cooling to 25 ℃ at a cooling rate of 400 ℃/min and keeping for 5 minutes; finally, heating to 290 ℃ at a speed of 10 ℃/min, keeping for 5 minutes, and then cooling to 100 ℃ at a speed of 10 ℃/min;
(3) and after the test is finished, storing the test data and the chart, analyzing and evaluating the post-processing performance of the sample, and optimizing the direction of the processing technological parameters.
Further, the sample to be evaluated can be colored POY or terylene slices dried at different drying temperatures.
Further, the data of the test required for evaluation of the post-processability of the colored POY are the heat of fusion Δ Hm, the heat of cold crystallization Δ Hc, and the heat of fusion Δ Ho of 100% crystalline PET (126.9J/g).
Further, the method for evaluating the post-processing performance of the colored POY comprises the following steps: degree of crystallinity X according to DSCDSCCalculating by the formula: xDSCThe post-processability of the colored POY having low crystallinity is better when the ratio is (Δ Hm- Δ Hc)/Δ Ho × 100%.
Furthermore, the data of the test required by the evaluation of the post-processing performance of the polyester slices dried at different drying temperatures are thermal crystallization peak temperature Tmc (DEG C), thermal crystallization peak temperature width Delta T (DEG C) and exothermic crystallization amount Delta H (J/g).
Further, the method for evaluating the post-processing performance of the polyester chips dried at different drying temperatures and optimizing the processing technological parameters comprises the following steps: the method comprises the steps of determining numerical values of a thermal crystallization peak temperature, a thermal crystallization rate and a crystallization interval from a calculation result of a differential scanning calorimeter, firstly comparing the thermal crystallization peak temperatures of the polyester slices dried at different drying temperatures, wherein the lower the thermal crystallization peak temperature is, the better the post-processing performance is, comparing the thermal crystallization rate with the crystallization interval if the thermal crystallization peak temperatures are the same, the slower the thermal crystallization rate is, the narrower the crystallization interval is, the better the post-processing performance is, and reversely determining the optimal drying temperature of the polyester slices according to an evaluation result of the post-processing performance.
By the scheme, the invention at least has the following advantages:
1. the invention adopts DSC (differential scanning calorimetry) analysis to test the crystallization performance of POY protofilament, fully simulates two processes of thermal crystallization and cold crystallization of high polymer in the false twisting process of POY, and evaluates the quality of POY, especially the quality of processability through the analysis of crystallization temperature and crystallization rate numerical value, compared with the traditional national standard, the invention characterizes, verifies or conjectures the product quality from the side, the evaluation of the invention is more accurate, otherwise, the invention seeks transverse and longitudinal differences, optimizes process parameters and improves definite direction and trend;
2. the method adopts DSC (differential scanning calorimetry) analysis to test the crystallization performance of the dried slices, and evaluates the drying effect of the slices through the high and low crystallization temperatures and the high and low crystallization rates.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is a DSC measurement profile of example 1;
fig. 2, 3 and 4 are DSC measurement maps of example 2.
Detailed Description
A method for evaluating spinning post-processing performance based on differential scanning calorimetry is characterized in that the differential scanning calorimetry technology is combined with calculation of a thermal analysis kinetic theory formula to evaluate the spinning post-processing performance, and the method comprises the following specific steps:
(1) cutting 8-10 mg of a sample to be evaluated into pieces, putting the pieces into a sample vessel, and putting the sample vessel into a differential scanning calorimeter;
(2) performing DSC measurement by using a differential scanning calorimeter, wherein the atmosphere is N2, the flow rate is 20ml/min, the heating rate is set to 10 ℃/min, the temperature is increased to 290 ℃, and the temperature is kept for 5 min; then cooling to 25 ℃ at a cooling rate of 400 ℃/min and keeping for 5 minutes; finally, the temperature is increased to 290 ℃ at the speed of 10 ℃/min, kept for 5 minutes and then reduced to 100 ℃ at the speed of 10 ℃/min.
(3) And after the test is finished, storing the test data and the chart, analyzing and evaluating the post-processing performance of the sample, and optimizing the direction of the processing technological parameters.
Preferably, the sample to be evaluated can be colored POY or terylene slices dried at different drying temperatures. Preferably, the data of the test required for the evaluation of the post-processability of the colored POY are the heat of fusion Δ Hm, the heat of cold crystallization Δ Hc, and the heat of fusion Δ Ho of 100% crystalline PET (126.9J/g). Preferably, the method for evaluating the post-processing performance of the colored POY comprises the following steps: degree of crystallinity X according to DSCDSCCalculating by the formula: xDSCThe post-processability of the colored POY having low crystallinity is better when the ratio is (Δ Hm- Δ Hc)/Δ Ho × 100%. Preferably, the data of the test required for evaluating the post-processing performance of the polyester chips dried at different drying temperatures are thermal crystallization peak temperature Tmc (DEG C), thermal crystallization peak temperature width Delta T (DEG C), and exothermic crystallization amount Delta H (J/g). Preferably, the method for evaluating the post-processing performance of the polyester chips dried at different drying temperatures and optimizing the processing technological parameters comprises the following steps: the method comprises the steps of determining numerical values of a thermal crystallization peak temperature, a thermal crystallization rate and a crystallization interval from a calculation result of a differential scanning calorimeter, firstly comparing the thermal crystallization peak temperatures of the polyester slices dried at different drying temperatures, wherein the lower the thermal crystallization peak temperature is, the better the post-processing performance is, comparing the thermal crystallization rate with the crystallization interval if the thermal crystallization peak temperatures are the same, the slower the thermal crystallization rate is, the narrower the crystallization interval is, the better the post-processing performance is, and reversely determining the optimal drying temperature of the polyester slices according to an evaluation result of the post-processing performance.
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
A method for evaluating spinning post-processing performance based on differential scanning calorimetry is characterized in that the differential scanning calorimetry technology is combined with calculation of a thermal analysis kinetic theory formula to evaluate the spinning post-processing performance, and the method comprises the following specific steps:
(1) cutting a certain amount of 8-10 mg colored POY for vehicles into pieces, putting the pieces into a sample vessel, and putting the sample vessel into a differential scanning calorimeter;
(2) performing DSC measurement by using a differential scanning calorimeter, wherein the atmosphere is N2, the flow rate is 20ml/min, the heating rate is set to 10 ℃/min, the temperature is increased to 290 ℃, and the temperature is kept for 5 min; then cooling to 25 ℃ at a cooling rate of 400 ℃/min and keeping for 5 minutes; finally, the temperature is increased to 290 ℃ at the speed of 10 ℃/min, kept for 5 minutes and then reduced to 100 ℃ at the speed of 10 ℃/min.
(3) And after the test is finished, storing the test data and the chart, analyzing and evaluating the post-processing performance of the sample, and optimizing the direction of the processing technological parameters.
The crystallinity is an important structural parameter for representing high polymers, and the crystallinity of the colored POY for the vehicle is important for the smooth performance of DTY processing and the quality of the performance of finished products. However, the measurement of crystallinity is a complicated problem in theory and practice because the boundary between the crystalline region and the amorphous region is not clear. Differential scanning differential thermal analysis (DSC) is a rapid and easy method for determining the degree of crystallinity of POY. The heat of fusion of the polymer is proportional to the degree of crystallinity, and for low-crystalline POY filaments, the degree of crystallinity of DSC can be calculated using the following formula.
XDSC＝(ΔHm-ΔHc)/ΔHo×100％
Wherein: Δ Hm is the heat of fusion,. DELTA.Hc is the heat of cold crystallization,. DELTA.Ho is the heat of fusion (126.9J/g) of 100% crystalline PET
The following table shows the results of DSC tests performed on POY of the same specification and pigment addition under two different process conditions:
| test items | Unit of | POYA | POYB |
| ΔHm | J/g | 46.63 | 49.22 |
| ΔHc | J/g | 28.95 | 28.66 |
| XDSC | ％ | 13.93％ | 16.20％ |
Due to the pre-melting phenomenon, the actual crystallinity of POY may deviate from the calculated data. But under the same test conditions, the yarn POYBDegree of crystallinity ratio POYAHigh means POYBThe primary structure is relatively perfect, which is not beneficial to the formation of new molecular structure in the false twisting process and has negative influence on the uniformity of DTY quality. Thus, from the numerical value of crystallinity, POYAThe processability is better.
Example 2
A method for evaluating spinning post-processing performance based on differential scanning calorimetry is characterized in that the differential scanning calorimetry technology is combined with calculation of a thermal analysis kinetic theory formula to evaluate the spinning post-processing performance, and the method comprises the following specific steps:
(1) (1) cutting a certain amount of 8-10 mg of colored POY for vehicles into pieces, putting the pieces into a sample vessel, and putting the sample vessel into a differential scanning calorimeter;
(2) performing DSC measurement by using a differential scanning calorimeter, wherein the atmosphere is N2, the flow rate is 20ml/min, the heating rate is set to 10 ℃/min, the temperature is increased to 290 ℃, and the temperature is kept for 5 min; then cooling to 25 ℃ at a cooling rate of 400 ℃/min and keeping for 5 minutes; finally, heating to 290 ℃ at a speed of 10 ℃/min, keeping for 5 minutes, and then cooling to 100 ℃ at a speed of 10 ℃/min;
(3) and after the test is finished, storing the test data and the chart, analyzing and evaluating the post-processing performance of the sample, and optimizing the direction of the processing technological parameters.
The polymer generates heat because of crystallization during constant temperature rising and constant temperature falling of the melt, and an exothermic peak is formed, wherein the former is cold crystallization peak temperature Tc, the latter is hot crystallization peak temperature Tmc, and Tc and Tmc are phase transition temperatures related to the crystallization process of the high polymer. Tmc is related to the ease with which the polymer molecules nucleate, the higher the Tmc, the more efficiently the polymer can nucleate at higher temperatures. The constant-speed temperature reduction process of the self-melt in DSC is close to the cooling process of the spinning melt, so that the chips with high thermal crystallization temperature and high crystallization rate are not beneficial to the stable running of the spinning process and the improvement of the POY quality.
In practice, we selected three sections at drying temperature and performed DSC test as follows:
in the table, it is seen that at the drying temperature of 166 ℃, the difference of the thermal crystallization temperature in the slice spinning cooling process is not large at a higher temperature, but the thermal crystallization rate is slow, the crystallization interval is narrow, which is more beneficial to the structure forming and the improvement of fiber performance, and the drying temperature of 166 ℃ is selected in the actual production.
The working principle of the invention is as follows:
1. the invention adopts DSC (differential scanning calorimetry) analysis to test the crystallization performance of POY protofilament, fully simulates two processes of thermal crystallization and cold crystallization of high polymer in the false twisting process of POY, and evaluates the quality of POY, especially the quality of processability through the analysis of crystallization temperature and crystallization rate numerical value, compared with the traditional national standard, the invention characterizes, verifies or conjectures the product quality from the side, the evaluation of the invention is more accurate, otherwise, the invention seeks transverse and longitudinal differences, optimizes process parameters and improves definite direction and trend;
2. the method adopts DSC (differential scanning calorimetry) analysis to test the crystallization performance of the dried slices, and evaluates the drying effect of the slices through the high and low crystallization temperatures and the high and low crystallization rates.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A method for evaluating the processability after spinning based on differential scanning calorimetry is characterized in that: the method is to combine differential scanning calorimeter technology with thermal analysis kinetic theory formula calculation to evaluate the post-processing performance of spinning, and comprises the following specific steps:
(1) cutting 8-10 mg of a sample to be evaluated into pieces, putting the pieces into a sample vessel, and putting the sample vessel into a differential scanning calorimeter;
(2) performing DSC measurement by using a differential scanning calorimeter, introducing nitrogen at a flow rate of 20ml/min for protection, setting a heating rate of 10 ℃/min, heating to 290 ℃, and keeping for 5 min; then cooling to 25 ℃ at a cooling rate of 400 ℃/min and keeping for 5 minutes; finally, heating to 290 ℃ at a speed of 10 ℃/min, keeping for 5 minutes, and then cooling to 100 ℃ at a speed of 10 ℃/min;
(3) and after the test is finished, storing the test data and the chart, analyzing and evaluating the post-processing performance of the sample, and optimizing the direction of the processing technological parameters.
2. The method for evaluating the processability after spinning based on differential scanning calorimetry as claimed in claim 1, wherein: the sample to be evaluated can be colored POY or terylene slices dried at different drying temperatures.
3. The method for evaluating the processability after spinning based on differential scanning calorimetry as claimed in claim 2, wherein: the data of the tests required for the evaluation of the post-processability of the colored POY are the heat of fusion Δ Hm, the heat of cold crystallization Δ Hc, and the heat of fusion Δ Ho of 100% crystalline PET (126.9J/g).
4. The method for evaluating processability after spinning based on differential scanning calorimetry as claimed in claim 1 or 2Characterized in that: the method for evaluating the post-processing performance of the colored POY comprises the following steps: degree of crystallinity X according to DSCDSCCalculating by the formula: xDSCThe post-processability of the colored POY having low crystallinity is better when the ratio is (Δ Hm- Δ Hc)/Δ Ho × 100%.
5. The method for evaluating the processability after spinning based on differential scanning calorimetry as claimed in claim 2, wherein: the data of the test required by the evaluation of the post-processing performance of the polyester slices dried at different drying temperatures are thermal crystallization peak temperature Tmc (DEG C), thermal crystallization peak temperature width Delta T (DEG C) and exothermic crystallization amount Delta H (J/g).
6. The method for evaluating processability after spinning based on differential scanning calorimetry according to claim 1 or 2, wherein: the method for evaluating the post-processing performance of the polyester chips dried at different drying temperatures and optimizing the processing technological parameters comprises the following steps: the method comprises the steps of determining numerical values of a thermal crystallization peak temperature, a thermal crystallization rate and a crystallization interval from a calculation result of a differential scanning calorimeter, firstly comparing the thermal crystallization peak temperatures of the polyester slices dried at different drying temperatures, wherein the lower the thermal crystallization peak temperature is, the better the post-processing performance is, comparing the thermal crystallization rate with the crystallization interval if the thermal crystallization peak temperatures are the same, the slower the thermal crystallization rate is, the narrower the crystallization interval is, the better the post-processing performance is, and reversely determining the optimal drying temperature of the polyester slices according to an evaluation result of the post-processing performance.
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