CN112345478A - Method for testing content of residual dimethyl sulfoxide in polyacrylonitrile protofilament - Google Patents
Method for testing content of residual dimethyl sulfoxide in polyacrylonitrile protofilament Download PDFInfo
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- CN112345478A CN112345478A CN202011086913.1A CN202011086913A CN112345478A CN 112345478 A CN112345478 A CN 112345478A CN 202011086913 A CN202011086913 A CN 202011086913A CN 112345478 A CN112345478 A CN 112345478A
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- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 title claims abstract description 206
- 229920002239 polyacrylonitrile Polymers 0.000 title claims abstract description 108
- 238000012360 testing method Methods 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 138
- 239000000243 solution Substances 0.000 claims abstract description 34
- 238000002156 mixing Methods 0.000 claims abstract description 26
- 239000012088 reference solution Substances 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims description 36
- 239000007788 liquid Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 24
- 239000000835 fiber Substances 0.000 abstract description 18
- 238000010521 absorption reaction Methods 0.000 abstract description 12
- 238000000605 extraction Methods 0.000 abstract description 11
- 238000000354 decomposition reaction Methods 0.000 abstract description 5
- 239000000284 extract Substances 0.000 abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 40
- 230000000052 comparative effect Effects 0.000 description 12
- 235000019441 ethanol Nutrition 0.000 description 12
- 239000007864 aqueous solution Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 229920000049 Carbon (fiber) Polymers 0.000 description 5
- 239000004917 carbon fiber Substances 0.000 description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 5
- 239000013557 residual solvent Substances 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000002798 spectrophotometry method Methods 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- HHVIBTZHLRERCL-UHFFFAOYSA-N sulfonyldimethane Chemical compound CS(C)(=O)=O HHVIBTZHLRERCL-UHFFFAOYSA-N 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 238000003811 acetone extraction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000006286 aqueous extract Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- LBOVMDOAMWYGHK-UHFFFAOYSA-N ethanol;methylsulfinylmethane Chemical compound CCO.CS(C)=O LBOVMDOAMWYGHK-UHFFFAOYSA-N 0.000 description 1
- 239000000469 ethanolic extract Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- VCCPBPXMXHHRLN-UHFFFAOYSA-N methylsulfinylmethane;propan-2-one Chemical compound CC(C)=O.CS(C)=O VCCPBPXMXHHRLN-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N2021/3196—Correlating located peaks in spectrum with reference data, e.g. fingerprint data
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Abstract
The invention discloses a method for testing the content of residual dimethyl sulfoxide in polyacrylonitrile protofilament, which comprises the following steps: (1) mixing and oscillating polyacrylonitrile protofilament and acetone at 30-50 ℃ so as to leach residual dimethyl sulfoxide in the polyacrylonitrile protofilament into the acetone; (2) and (2) testing the acetone solution containing the dimethyl sulfoxide obtained in the step (1) by using an ultraviolet spectrophotometer by taking acetone as a reference solution, and calculating the content of the residual dimethyl sulfoxide in the polyacrylonitrile protofilament. The method adopts acetone as an extractant of dimethyl sulfoxide in the polyacrylonitrile protofilament, can extract the dimethyl sulfoxide in the protofilament at a lower temperature, avoids the decomposition of the dimethyl sulfoxide, has better wettability to PAN fibers than water, has higher extraction efficiency, and has more sensitive ultraviolet absorption of the dimethyl sulfoxide in the acetone.
Description
Technical Field
The invention belongs to the field of fibers, and particularly relates to a method for testing the content of residual dimethyl sulfoxide in polyacrylonitrile protofilament.
Background
High-performance Polyacrylonitrile (PAN) based carbon fiber is widely applied to the fields of aviation, aerospace, automobiles, energy sources, sports equipment and the like, and is a military and civil dual-purpose key material closely related to national economy and national defense safety. PAN precursor for carbon fiber is prepared by solution spinning, and then carbon fiber is obtained by preoxidation carbonization. Dimethyl sulfoxide is a good solvent of polyacrylonitrile solution and is also a common spinning solvent. The polyacrylonitrile solution is solidified and formed to obtain fibrous nascent fiber, and the polyacrylonitrile protofilament is prepared through the processes of drafting, washing, oiling, drying densification, heat setting and the like. If the washing process is imperfect, the solvent dimethyl sulfoxide residue exists in the fiber, when the dimethyl sulfoxide residue in the polyacrylonitrile precursor is high, the structure and the performance of the precursor and the stable operation of the pre-oxidation carbonization heat treatment process are influenced, and therefore, the content of the dimethyl sulfoxide residue solvent is an important index for controlling the quality of the polyacrylonitrile precursor product for the carbon fiber.
At present, the content of dimethyl sulfoxide in polyacrylonitrile protofilament cannot be directly measured, FZ1573-2015 proposes that dimethyl sulfoxide in PAN fiber is extracted by boiling point or near-boiling point water, then the concentration of dimethyl sulfoxide in aqueous solution is measured by adopting instrument analysis methods such as ultraviolet spectrophotometry, gas chromatography and liquid chromatography, and then the content of residual solvent in fiber is calculated. Dimethyl sulfoxide has a boiling point of 189 ℃, but thermal reaction occurs at 60 ℃ or higher to generate dimethyl sulfide, dimethyl sulfone, dimethyl disulfide and the like, and particularly, when the polyacrylonitrile fiber is heated for 1 hour at 100 ℃ under an acidic condition, the decomposition rate is about 13%, and acidic comonomers are often present in the polyacrylonitrile fiber. Aiming at the problem that water with a near boiling point is commonly used as an extracting agent in domestic production enterprises and scientific research institutions at the present stage, the extraction temperature and the acidic atmosphere decompose the residual dimethyl sulfoxide in the fiber to be detected, so that the extracted substance dimethyl sulfoxide is changed, the influence on the residual dimethyl sulfoxide in the fiber is negligible when the content of the residual dimethyl sulfoxide in the fiber is high, but the influence on the pretreatment caused by the low content of the residual solvent in the domestic carbon fiber precursor at the present stage cannot be ignored.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for testing the content of the residual dimethyl sulfoxide in the polyacrylonitrile precursor, which adopts acetone as an extractant of the dimethyl sulfoxide in the polyacrylonitrile precursor, can extract the dimethyl sulfoxide in the precursor at a lower temperature, avoids the decomposition of the dimethyl sulfoxide, has better wettability to PAN fibers than water, has higher extraction efficiency, and has more sensitive ultraviolet absorption of the dimethyl sulfoxide in the acetone.
The invention provides a method for testing the content of residual dimethyl sulfoxide in polyacrylonitrile protofilament. According to an embodiment of the invention, the method comprises: (1) mixing and oscillating polyacrylonitrile protofilament and acetone at 30-50 ℃ so as to leach residual dimethyl sulfoxide in the polyacrylonitrile protofilament into the acetone; (2) and (2) testing the acetone solution containing the dimethyl sulfoxide obtained in the step (1) by using an ultraviolet spectrophotometer by taking acetone as a reference solution, and calculating the content of the residual dimethyl sulfoxide in the polyacrylonitrile protofilament.
Optionally, in the step (1), the solid-to-liquid ratio of the polyacrylonitrile protofilament to the acetone is (0.5-1.5) g: 100 mL.
Optionally, in the step (1), the polyacrylonitrile protofilament and the acetone are mixed and shaken for 30-60 minutes at 30-50 ℃.
Optionally, in the step (2), the testing wavelength of the ultraviolet spectrophotometer is 190-250 nm.
Compared with the prior art, the method adopts acetone as an extracting agent, the acetone and the dimethyl sulfoxide can be mutually dissolved in any proportion, the polyacrylonitrile protofilament and the acetone are mixed and oscillated at 30-50 ℃, the dimethyl sulfoxide in the polyacrylonitrile protofilament can be leached into an acetone solvent, the dimethyl sulfoxide is prevented from being decomposed by low-temperature extraction, the PAN fiber is better in wettability of the acetone than water, the extraction efficiency is higher, then an ultraviolet spectrophotometer is adopted to determine the content of the dimethyl sulfoxide in the acetone, the ultraviolet absorption of the dimethyl sulfoxide in the acetone is more sensitive, and compared with the existing extraction and test method, the method does not generate the decomposition of the dimethyl sulfoxide in the extraction process, so that the test result is more accurate, and the accurate content information of the dimethyl sulfoxide residual solvent in the protofilament can be obtained.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a UV absorption spectrum of an acetone extraction solution and a dimethylsulfoxide acetone solution of examples 1-4;
FIG. 2 is a UV absorption spectrum of an aqueous extract solution and an aqueous solution of dimethyl sulfoxide of comparative examples 1 to 4;
FIG. 3 is an ultraviolet absorption spectrum of the ethanol extract solution and the dimethylsulfoxide ethanol solution of comparative examples 5 to 8.
Detailed Description
The present invention will be further described with reference to the following examples, which are illustrative only and not intended to be limiting, and the scope of the present invention is not limited thereby.
The invention provides a method for testing the content of residual dimethyl sulfoxide in polyacrylonitrile protofilament. According to an embodiment of the invention, the method comprises:
s1: mixing and oscillating polyacrylonitrile protofilament and acetone at 30-50 DEG C
In this step, mix the vibration with polyacrylonitrile protofilament and acetone under 30 ~ 50 ℃, acetone and dimethyl sulfoxide can be soluble each other with arbitrary proportion, thereby can be with the dimethyl sulfoxide in the polyacrylonitrile protofilament extract in the acetone, and the mixed vibration of this application is gone on under 30 ~ 50 ℃ of temperature, it decomposes to have avoided dimethyl sulfoxide to take place, and acetone is better than water to PAN fibre infiltration nature (adopt Wilhelmy method test acetone and PAN fibre contact angle and be less than water and PAN fibre contact angle, acetone and polyacrylonitrile protofilament's contact angle is less than 51.1 degree, water and polyacrylonitrile protofilament's contact angle is 73.9 degrees), and extraction efficiency is higher. Further, in the mixing oscillation process, the solid-to-liquid ratio of the polyacrylonitrile protofilament to the acetone is (0.5-1.5) g: 100 mL. The inventor finds that if the mass of the polyacrylonitrile protofilament is too small, on one hand, the weighing error is large, and on the other hand, the content of dimethyl sulfoxide which is leached into an acetone solvent is too small, so that a large error is caused during ultraviolet spectrophotometry; if the mass of the polyacrylonitrile protofilament is too large, the liquid-solid ratio is relatively small, and the dimethyl sulfoxide in the fiber can not be completely eluted by acetone. Meanwhile, the polyacrylonitrile protofilament and acetone are mixed and oscillated for 30-60 minutes at 30-50 ℃.
S2: testing the acetone solution containing the dimethyl sulfoxide obtained in the step (1) by using an ultraviolet spectrophotometer by taking acetone as a reference solution
In the step, acetone is used as a reference solution, an ultraviolet spectrophotometer is used for testing the acetone solution containing the dimethyl sulfoxide obtained in the step S1, and the content of the residual dimethyl sulfoxide in the polyacrylonitrile protofilament is calculated. Specifically, the absorbance at the maximum absorption wavelength (determined by measuring an ultraviolet spectrum with the wavelength of 190-250 nm) is taken as a reference, the concentration of dimethyl sulfoxide in acetone is calculated according to a standard curve, and the content of the residual solvent dimethyl sulfoxide in the polyacrylonitrile protofilament is calculated according to the volume of the acetone and the mass of the polyacrylonitrile protofilament. Meanwhile, the inventor finds that the ultraviolet absorption coefficient of the dimethyl sulfoxide in the acetone is 2.50 multiplied by 10 by adopting the ultraviolet spectrophotometry4(cm3.g-1.cm-1) The ultraviolet absorption coefficient of dimethyl sulfoxide in water is 1.14X 104(cm3.g-1.cm-1) Namely, the ultraviolet absorption sensitivity of the dimethyl sulfoxide in the acetone is better than that of the dimethyl sulfoxide in the water.
The inventor finds that acetone is used as an extracting agent, the acetone and dimethyl sulfoxide can be mutually dissolved in any proportion, the polyacrylonitrile protofilament and the acetone are mixed and oscillated at the temperature of 30-50 ℃, the dimethyl sulfoxide in the polyacrylonitrile protofilament can be soaked into an acetone solution, the dimethyl sulfoxide is prevented from being decomposed, the acetone has better wettability to PAN fibers than water, the extraction efficiency is higher, then an ultraviolet spectrophotometer is used for measuring the content of the dimethyl sulfoxide in the acetone, the ultraviolet absorption of the dimethyl sulfoxide in the acetone is more sensitive, compared with the existing extraction and test method, the decomposition of the dimethyl sulfoxide cannot occur in the extraction process, the test result is more accurate, and accurate dimethyl sulfoxide residual solvent content information in the protofilament can be obtained.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and should not be construed as limiting the invention in any way.
Example 1
(1) Taking 5 groups of polyacrylonitrile protofilament in the same batch, and mixing the groups with acetone according to the solid-to-liquid ratio of 1.0 g: mixing and oscillating the polyacrylonitrile precursor solution for 60min at the temperature of 30 ℃ by 100mL, so that residual dimethyl sulfoxide in the polyacrylonitrile precursor is leached into acetone;
(2) and (3) testing the acetone solution containing the dimethyl sulfoxide obtained in the step (1) at the wavelength of 190-250 nm by using acetone as a reference solution by using an ultraviolet spectrophotometer, wherein the curve a in the figure 1 is shown, and calculating the content of the residual dimethyl sulfoxide in 5 groups of polyacrylonitrile protofilaments, and the specific test result is shown in table 1.
Example 2
(1) Taking 5 groups of polyacrylonitrile protofilament of the same batch of example 1 and acetone according to a solid-to-liquid ratio of 1.0 g: mixing and oscillating the polyacrylonitrile precursor solution for 50min at 40 ℃ by 100mL so as to leach residual dimethyl sulfoxide in the polyacrylonitrile precursor into acetone;
(2) and (3) testing the acetone solution containing the dimethyl sulfoxide obtained in the step (1) at the wavelength of 190-250 nm by using acetone as a reference solution by using an ultraviolet spectrophotometer, wherein the curve b in the figure 1 is shown, and calculating the content of the residual dimethyl sulfoxide in 5 groups of polyacrylonitrile protofilaments, and the specific test result is shown in table 1.
Example 3
(1) Taking 5 groups of polyacrylonitrile protofilament of the same batch of example 1 and acetone according to the solid-to-liquid ratio of 1.0 g: mixing and oscillating the polyacrylonitrile precursor solution for 40min at the temperature of 45 ℃ by 100mL, so that residual dimethyl sulfoxide in the polyacrylonitrile precursor is leached into acetone;
(2) and (3) testing the acetone solution containing dimethyl sulfoxide obtained in the step (1) by using acetone as a reference solution and an ultraviolet spectrophotometer at the wavelength of 190-250 nm, wherein the curve c in the figure 1 is shown, and calculating the content of the residual dimethyl sulfoxide in 5 groups of polyacrylonitrile protofilaments, and the specific test result is shown in table 1.
Example 4
(1) Taking 5 groups of polyacrylonitrile protofilament of the same batch of example 1 and acetone according to the solid-to-liquid ratio of 1.0 g: mixing and oscillating the polyacrylonitrile precursor solution for 30min at 50 ℃ by 100mL so as to leach residual dimethyl sulfoxide in the polyacrylonitrile precursor into acetone;
(2) and (3) testing the acetone solution containing the dimethyl sulfoxide obtained in the step (1) at the wavelength of 190-250 nm by using acetone as a reference solution by using an ultraviolet spectrophotometer, wherein the curve d in the figure 1 shows, and calculating the content of the residual dimethyl sulfoxide in 5 groups of polyacrylonitrile protofilaments, and the specific test result is shown in table 1.
Comparative example 1
(1) Taking 5 groups of polyacrylonitrile protofilament in the same batch as in example 1, and mixing the groups with water according to a solid-to-liquid ratio of 1.0 g: mixing and oscillating the polyacrylonitrile precursor solution for 60min at 50 ℃ by 100mL so as to leach residual dimethyl sulfoxide in the polyacrylonitrile precursor into water;
(2) and (2) testing the aqueous solution containing the dimethyl sulfoxide obtained in the step (1) at the wavelength of 190-250 nm by using water as a reference solution by using an ultraviolet spectrophotometer, wherein a dimethyl sulfoxide absorption peak does not appear at the position of 207nm, as shown in a curve a in fig. 2, the content of the residual dimethyl sulfoxide in the polyacrylonitrile protofilament cannot be calculated, and specific test results are shown in table 1.
Comparative example 2
(1) Taking 5 groups of polyacrylonitrile protofilament in the same batch as in example 1, and mixing the groups with water according to a solid-to-liquid ratio of 2.5 g: mixing and oscillating the polyacrylonitrile precursor solution for 60min at 50 ℃ by 100mL so as to leach residual dimethyl sulfoxide in the polyacrylonitrile precursor into water;
(2) and (2) testing the aqueous solution containing the dimethyl sulfoxide obtained in the step (1) at the wavelength of 190-250 nm by using water as a reference solution by using an ultraviolet spectrophotometer, wherein a dimethyl sulfoxide absorption peak does not appear at the position of 207nm, as shown in a curve b in fig. 2, the content of the residual dimethyl sulfoxide in the polyacrylonitrile protofilament cannot be calculated, and specific test results are shown in table 1.
Comparative example 3
(1) Taking 5 groups of polyacrylonitrile protofilament in the same batch as in example 1, and mixing the groups with water according to a solid-to-liquid ratio of 2.5 g: mixing and oscillating the polyacrylonitrile precursor solution for 60min at 100 ℃ by 100mL so as to leach residual dimethyl sulfoxide in the polyacrylonitrile precursor into water;
(2) and (3) testing the aqueous solution containing the dimethyl sulfoxide obtained in the step (1) at the wavelength of 190-250 nm by using water as a reference solution by using an ultraviolet spectrophotometer, wherein a dimethyl sulfoxide absorption shoulder appears at the position of 207nm, the content of the residual dimethyl sulfoxide in the polyacrylonitrile protofilament is calculated according to a curve c in a graph of fig. 2, and specific test results are shown in table 1.
Comparative example 4
(1) Taking 5 groups of polyacrylonitrile protofilament in the same batch as in example 1, and mixing the groups with water according to a solid-to-liquid ratio of 2.5 g: mixing and oscillating the polyacrylonitrile precursor solution for 120min at 100 ℃ by 100mL so as to leach residual dimethyl sulfoxide in the polyacrylonitrile precursor into water;
(2) and (3) testing the aqueous solution containing the dimethyl sulfoxide obtained in the step (1) at the wavelength of 190-250 nm by using water as a reference solution by using an ultraviolet spectrophotometer, wherein a dimethyl sulfoxide absorption shoulder appears at the position of 207nm, the content of the residual dimethyl sulfoxide in the polyacrylonitrile protofilament is calculated according to a curve d in a graph of fig. 2, and specific test results are shown in table 1.
Comparative example 5
(1) Taking 5 groups of polyacrylonitrile protofilament in the same batch as in example 1, and mixing the groups with absolute ethyl alcohol according to a solid-to-liquid ratio of 1.0 g: mixing and oscillating the polyacrylonitrile precursor solution for 60min at the temperature of 30 ℃ by 100mL, so that residual dimethyl sulfoxide in the polyacrylonitrile precursor is leached into ethanol;
(2) and (3) testing the ethanol solution containing the dimethyl sulfoxide obtained in the step (1) at the wavelength of 190-250 nm by using ethanol as a reference solution by using an ultraviolet spectrophotometer, wherein the curve a in the figure 3 shows, and calculating the content of the residual dimethyl sulfoxide in 5 groups of polyacrylonitrile protofilaments, and the specific test result is shown in table 1.
Comparative example 6
(1) Taking 5 groups of polyacrylonitrile protofilament in the same batch as in example 1, and mixing the groups with absolute ethyl alcohol according to a solid-to-liquid ratio of 1.0 g: mixing and oscillating the polyacrylonitrile precursor solution for 50min at 40 ℃ by 100mL so as to leach residual dimethyl sulfoxide in the polyacrylonitrile precursor into ethanol;
(2) and (3) testing the ethanol solution containing the dimethyl sulfoxide obtained in the step (1) at the wavelength of 190-250 nm by using an ultraviolet spectrophotometer by taking ethanol as a reference solution, wherein the curve b in the figure 3 is shown, and calculating the content of the residual dimethyl sulfoxide in 5 groups of polyacrylonitrile protofilaments, wherein the specific test result is shown in table 1.
Comparative example 7
(1) Taking 5 groups of polyacrylonitrile protofilament in the same batch as in example 1, and mixing the groups with absolute ethyl alcohol according to a solid-to-liquid ratio of 1.0 g: mixing and oscillating the polyacrylonitrile precursor solution for 40min at the temperature of 45 ℃ by 100mL, so that residual dimethyl sulfoxide in the polyacrylonitrile precursor is leached into ethanol;
(2) and (3) testing the ethanol solution containing the dimethyl sulfoxide obtained in the step (1) at the wavelength of 190-250 nm by using an ultraviolet spectrophotometer by taking ethanol as a reference solution, wherein the curve c in the figure 3 shows, and calculating the content of the residual dimethyl sulfoxide in 5 groups of polyacrylonitrile protofilaments, wherein the specific test result is shown in table 1.
Comparative example 8
(1) Taking 5 groups of polyacrylonitrile protofilament in the same batch as in example 1, and mixing the groups with absolute ethyl alcohol according to a solid-to-liquid ratio of 1.0 g: mixing and oscillating the polyacrylonitrile precursor solution for 30min at 50 ℃ by 100mL so as to leach residual dimethyl sulfoxide in the polyacrylonitrile precursor into ethanol;
(2) and (3) testing the ethanol solution containing the dimethyl sulfoxide obtained in the step (1) at the wavelength of 190-250 nm by using an ultraviolet spectrophotometer by taking ethanol as a reference solution, wherein the curve d in the figure 3 shows, and calculating the content of the residual dimethyl sulfoxide in 5 groups of polyacrylonitrile protofilaments, and the specific test result is shown in table 1.
TABLE 1 dimethyl sulfoxide content in Polyacrylonitrile precursor in examples 1-4 and comparative examples 1-8
Note: in comparative examples 1 to 2, the temperature was low, and therefore the residual dimethyl sulfoxide in the polyacrylonitrile precursor could hardly be washed out into water.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the technical principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (4)
1. A method for testing the content of residual dimethyl sulfoxide in polyacrylonitrile protofilament is characterized by comprising the following steps:
(1) mixing and oscillating polyacrylonitrile protofilament and acetone at 30-50 ℃ so as to leach residual dimethyl sulfoxide in the polyacrylonitrile protofilament into the acetone;
(2) and (2) testing the acetone solution containing the dimethyl sulfoxide obtained in the step (1) by using an ultraviolet spectrophotometer by taking acetone as a reference solution, and calculating the content of the residual dimethyl sulfoxide in the polyacrylonitrile protofilament.
2. The method according to claim 1, wherein in the step (1), the solid-to-liquid ratio of the polyacrylonitrile precursor to the acetone is (0.5-1.5) g: 100 mL.
3. The method according to claim 1 or 2, wherein in the step (1), the polyacrylonitrile precursor and the acetone are mixed and shaken at 30-50 ℃ for 30-60 minutes.
4. The method of claim 1, wherein in step (2), the test wavelength of the ultraviolet spectrophotometer is 190-250 nm.
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| CN202011086913.1A CN112345478B (en) | 2020-10-12 | 2020-10-12 | Method for testing content of residual dimethyl sulfoxide in polyacrylonitrile protofilament |
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| CN114216873A (en) * | 2021-12-15 | 2022-03-22 | 中复神鹰碳纤维股份有限公司 | Method for measuring impurity content of polyacrylonitrile polymer liquid |
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