CN101871887A - Method for on-line detection of coagulation bath concentration in production of polyacrylonitrile protofilament for carbon fiber - Google Patents
Method for on-line detection of coagulation bath concentration in production of polyacrylonitrile protofilament for carbon fiber Download PDFInfo
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- CN101871887A CN101871887A CN 201010210823 CN201010210823A CN101871887A CN 101871887 A CN101871887 A CN 101871887A CN 201010210823 CN201010210823 CN 201010210823 CN 201010210823 A CN201010210823 A CN 201010210823A CN 101871887 A CN101871887 A CN 101871887A
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- concentration
- dimethyl sulfoxide
- titer
- coagulating bath
- refraction index
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- 238000001514 detection method Methods 0.000 title claims abstract description 24
- 229920002239 polyacrylonitrile Polymers 0.000 title claims abstract description 18
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 17
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 17
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 230000015271 coagulation Effects 0.000 title abstract 4
- 238000005345 coagulation Methods 0.000 title abstract 4
- 238000000034 method Methods 0.000 title description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 108
- 239000012086 standard solution Substances 0.000 claims abstract description 9
- 230000001112 coagulating effect Effects 0.000 claims description 36
- 239000007788 liquid Substances 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 4
- 238000004891 communication Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000000007 visual effect Effects 0.000 abstract 1
- 238000007380 fibre production Methods 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 239000012286 potassium permanganate Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 238000004166 bioassay Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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- Treatment Of Fiber Materials (AREA)
Abstract
The invention relates to an on-line detection method for coagulation bath concentration in production of polyacrylonitrile protofilament for carbon fiber, which comprises the following steps: 1) preparing a dimethyl sulfoxide standard solution; 2) making a standard curve equation; 3) connecting equipment; 4) detecting on line; 5) the concentration was calculated. The invention solves the technical problems that the existing coagulation bath concentration detection method is long in time consumption, inaccurate in test result and incapable of realizing on-line detection. The invention is beneficial to improving the timeliness, the dynamic property and the control precision of the concentration control of the dimethyl sulfoxide in the coagulation bath. The testing method is rapid, accurate and visual, and is suitable for automatic production.
Description
Technical field
The invention belongs to field of measuring technique, be specifically related to coagulating bath concentration on-line detection method in a kind of polyacrylonitrile fibril for carbon fiber production.
Background technology
PAN-based carbon fiber has characteristics such as high specific strength, high ratio modulus, low-density, high temperature resistant, corrosion-resistant, creep resistant, stability are strong, in every field such as space flight and aviation, mechano-electronic, chemical building material, energy traffic boundless application is arranged all.The PAN-based carbon fiber production run comprises spinning solution polymerization, precursor production, precursor pre-oxidation and three links of charing, wherein precursor production is key link, and the quality quality of precursor and stability have decisive influence to the quality quality and the stability of final carbon fiber product.The production run of precursor mainly comprises spray silk, solidifies, drawing-off, wash, oil, the stages such as compacting by drying, relaxation heat setting.
Wherein process of setting is a very important process, this is a double diffusion process, the thread that spinneret orifice gushes out is uniform polyacrylonitrile true solution originally, coagulating bath then is the aqueous solution of dimethyl sulfoxide, when thread entered coagulating bath, the good solvent dimethyl sulfoxide concentration in the thread was greater than the dimethyl sulfoxide concentration in the coagulating bath; The water concentration of poor solvent water concentration in the thread in the coagulating bath.Therefore the factor of controlling double diffusion speed mainly comprises coagulating bath concentration, temperature, time etc.Because of the dimethyl sulfoxide in the thread constantly is diffused in the coagulating bath, and the water in the coagulating bath constantly is diffused in the thread, make the dimethyl sulfoxide concentration in the coagulating bath constantly change, therefore detect the concentration of dimethyl sulfoxide in the coagulating bath fast and accurately, and then continuous make-up water or low concentration dimethyl sulfoxide aqueous solution, stability of concentration with the maintenance coagulating bath is very important, thereby guarantees double diffused homogeneity.
How to measure in the past, at first dimethyl sulfoxide was oxidized to sulfone, made the manganese dioxide reduction of excessive potassium permanganate and generation again with potassium iodide, at last the iodine of separating out with the sodium thiosulfate titration with superfluous potassium permanganate with titrimetry.The advantage of this method do not need to be expensive detection equipment, can finish with simple Experimental Establishment, but also have following defective: 1, the consuming time of titrimetry had relatively high expectations than length and to the operator, operator's subjectivity is bigger to result's influence, and is unfavorable for the process control of coagulating bath concentration in the polyacrylonitrile fibril production run; 2, traditional chemical method can not be carried out online detection, can't control automatically.
Summary of the invention
The object of the invention provide a kind of polyacrylonitrile fibril for carbon fiber produce in the coagulating bath concentration on-line detection method, it has solved existing coagulating bath concentration detection method length consuming time, test result is inaccurate and the technical matters that can't realize online detection.
Technical solution of the present invention is:
Coagulating bath concentration on-line detection method during a kind of polyacrylonitrile fibril for carbon fiber is produced, its special character is: may further comprise the steps:
1] preparation dimethyl sulfoxide titer:
Identical raw material is prepared the dimethyl sulfoxide titer of a plurality of variable concentrations in the production of employing polyacrylonitrile fibril for carbon fiber;
2] production standard curvilinear equation:
Use refractometer to measure the refraction index of each dimethyl sulfoxide titer, draw dimethyl sulfoxide titer refraction index-dimethyl sulfoxide concentration of standard solution typical curve, obtain typical curve equation: Y=aX+b, wherein Y is a dimethyl sulfoxide titer refraction index, and X is the dimethyl sulfoxide concentration of standard solution; The typical curve equation is kept in the computer workstation;
3] connection device:
Online refractometer of series connection on the recycle feed pipe of coagulating bath or discharge nozzle, described online refractometer and computer workstation real-time Communication for Power;
4] online detection:
Online refractometer carries out online continuously refraction index to the dimethyl sulfoxide titer in coagulating bath recycle feed pipe or the discharge nozzle to be measured, and exports to computer workstation;
5] calculating concentration:
Computer workstation goes out the concentration and the output of dimethyl sulfoxide in the coagulating bath with the refraction index that receives by the typical curve Equation for Calculating.
The concentration requirement of the dimethyl sulfoxide titer of above-mentioned a plurality of variable concentrations is as follows: the round values of establishing dimethyl sulfoxide concentration value in the tested coagulating bath is α %, then the quantity of the dimethyl sulfoxide titer of the variable concentrations of being prepared is the odd number more than 7 and 7, one of them is α %, the numerical value of all the other half concentration standard liquid is less than α %, and the numerical value of the concentration standard liquid of half is greater than α % in addition; Spacing between two adjacent concentration of standard solution numerical value is 0.01 * α %～0.05 * α %.
The invention has the beneficial effects as follows: the present invention is by online refractometer of series connection on the recycle feed pipe of coagulating bath or discharge nozzle, by the typical curve of drawing standard dimethyl sulfoxide concentration and refraction index and the typical curve equation calculates dimethyl sulfoxide by the refraction index of measurement concentration.The present invention can be used for the on-line quick detection of dimethyl sulfoxide concentration in the coagulating bath of polyacrylonitrile fibril for carbon fiber production run, helps improving promptness, dynamic and the control accuracy of dimethyl sulfoxide concentration control in the coagulating bath.Method of testing of the present invention fast, accurately, intuitively is fit to carry out automated production.
Embodiment
Below the present invention is described in further details.The present invention is a coagulating bath concentration on-line detection method during a kind of polyacrylonitrile fibril for carbon fiber is produced, and it is as follows that it specifically detects step:
1) preparation dimethyl sulfoxide titer: the dimethyl sulfoxide titer that adopts raw material preparation variable concentrations identical in the polyacrylonitrile fibril for carbon fiber production; If the round values of dimethyl sulfoxide concentration value is α % in the tested coagulating bath, the quantity of the concentration standard liquid of then being prepared be 7 and more than, one of them is α %, the numerical value of all the other half concentration standard liquid is less than α %, the numerical value of the concentration standard liquid of half is greater than α % in addition; Spacing between two adjacent concentration of standard solution numerical value is 0.01 * α %～0.05 * α % (deriving from table 1); The concentration value X of the dimethyl sulfoxide concentration titer of preparing
0Expression.
2) measure the refraction index value Y of each titer
0Mensuration: use refractometer to measure the refraction index Y of dimethyl sulfoxide titer
0, draw refraction index-concentration standard curve, obtain straight-line equation, standard deviation S D and the degree of correlation RD of dimethyl sulfoxide concentration and refraction index, the typical curve equation is: Y=aX+b;
In the formula, Y is a refraction index, and X is a dimethyl sulfoxide concentration; A is a rate of curve, and b is the intercept of curve in Y-axis; The typical curve equation is stored on the computer workstation.
3) online detection: at coagulating bath recycle feed pipe or online refractometer of discharge nozzle place series connection, online refractometer carries out continuous on-line detection to the dimethyl sulfoxide in coagulating bath recycle feed pipe or the discharge nozzle, the refraction index of measuring is transferred to computer workstation, computer workstation is directly exported the concentration value of dimethyl sulfoxide by storing the calculating of typical curve equation within it.
Employed online refractometer is commercially available finished product, for example, can use the UR24 or the online refractometer of UR19 of Italian Ma Sali company.
Embodiment
The online detection of dimethyl sulfoxide concentration in certain production line coagulating bath
1) preparation dimethyl sulfoxide titer: the dimethyl sulfoxide titer that adopts raw material preparation variable concentrations identical in the polyacrylonitrile fibril for carbon fiber production; If the round values of dimethyl sulfoxide concentration value is α % in the tested coagulating bath, 7 of the quantity of the concentration standard liquid of then being prepared and more than, one of them is α %, the numerical value of all the other half concentration standard liquid is less than α %, the numerical value of the concentration standard liquid of half is greater than α % in addition
Spacing between two adjacent concentration of standard solution numerical value is 0.01 * α %～0.05 * α %; Select 11 points in this example for use, particular content sees Table 1.
2) the refraction index value Y of bioassay standard liquid
0Mensuration: use refractometer to measure the refraction index Y of dimethyl sulfoxide titer
0, test result sees Table 2.Draw refraction index-concentration standard curve, obtain the straight-line equation of dimethyl sulfoxide concentration and refraction index, this typical curve equation is: Y=0.01397X+1.31659, in the formula, Y is a refraction index, and X is a dimethyl sulfoxide concentration, its standard deviation S D be 0.9999 and degree of correlation RD be 1.38E-4.
The concentration of table 1 dimethyl sulfoxide titer
| Sample number into spectrum | Concentration (%) |
| ??1 | ??50.07％ |
| ??2 | ??51.95％ |
| ??3 | ??54.05％ |
| ??4 | ??56.08％ |
| ??5 | ??57.96％ |
| ??6 | ??60.01％ |
| ??7 | ??62.04％ |
| ??8 | ??63.99％ |
| ??9 | ??62.03％ |
| ??10 | ??59.92％ |
| ??11 | ??58.01％ |
The refraction index of table 2 titer
| Sample number into spectrum | Concentration (%) | Refraction index |
| ??1 | ??50.07％ | ??1.34463 |
| ??2 | ??51.95％ | ??1.35855 |
| ??3 | ??54.05％ | ??1.37243 |
| ??4 | ??56.08％ | ??1.38644 |
| ??5 | ??57.96％ | ??1.40027 |
| ??6 | ??60.01％ | ??1.41415 |
| ??7 | ??62.04％ | ??1.42858 |
| ??8 | ??63.99％ | ??1.44236 |
| ??9 | ??66.03％ | ??1.45645 |
| ??10 | ??67.92％ | ??1.47019 |
| ??11 | ??70.01％ | ??1.48427 |
3) online detection: online refractometer carries out continuous on-line detection to the dimethyl sulfoxide in coagulating bath recycle feed pipe or the discharge nozzle, directly exports the concentration value of dimethyl sulfoxide.Following table 3 is gathering of one group of online detection data of different time.
Table 3 test result
| Sample number into spectrum | Concentration (%) | Refraction index |
| Time 1 | ??60.55％ | ??1.32505 |
| Time 2 | ??60.93％ | ??1.32510 |
| Time 3 | ??61.76％ | ??1.32522 |
| Time 4 | ??62.09％ | ??1.32526 |
| Time 5 | ??62.47％ | ??1.32532 |
| Time 6 | ??62.90％ | ??1.32538 |
| Time 7 | ??63.18％ | ??1.32542 |
| Sample number into spectrum | Concentration (%) | Refraction index |
| Time 8 | ??63.55％ | ??1.32547 |
Claims (2)
1. coagulating bath concentration on-line detection method during a polyacrylonitrile fibril for carbon fiber is produced is characterized in that: may further comprise the steps:
1] preparation dimethyl sulfoxide titer:
Identical raw material is prepared the dimethyl sulfoxide titer of a plurality of variable concentrations in the production of employing polyacrylonitrile fibril for carbon fiber;
2] production standard curvilinear equation:
Use refractometer to measure the refraction index of each dimethyl sulfoxide titer, draw dimethyl sulfoxide titer refraction index-dimethyl sulfoxide concentration of standard solution typical curve, obtain typical curve equation: Y=aX+b, wherein Y is a dimethyl sulfoxide titer refraction index, and X is the dimethyl sulfoxide concentration of standard solution; The typical curve equation is kept in the computer workstation;
3] connection device:
Online refractometer of series connection on the recycle feed pipe of coagulating bath or discharge nozzle, described online refractometer and computer workstation real-time Communication for Power;
4] online detection:
Online refractometer carries out online continuously refraction index to the dimethyl sulfoxide titer in coagulating bath recycle feed pipe or the discharge nozzle to be measured, and exports to computer workstation;
5] calculating concentration:
Computer workstation goes out the concentration and the output of dimethyl sulfoxide in the coagulating bath with the refraction index that receives by the typical curve Equation for Calculating.
2. coagulating bath concentration on-line detection method during polyacrylonitrile fibril for carbon fiber according to claim 1 is produced, it is characterized in that: the concentration requirement of the dimethyl sulfoxide titer of described a plurality of variable concentrations is as follows: the round values of establishing dimethyl sulfoxide concentration value in the tested coagulating bath is α %, then the quantity of the dimethyl sulfoxide titer of the variable concentrations of being prepared is the odd number more than 7 and 7, one of them is α %, the numerical value of all the other half concentration standard liquid is less than α %, and the numerical value of the concentration standard liquid of half is greater than α % in addition; Spacing between two adjacent concentration of standard solution numerical value is 0.01 * α %～0.05 * α %.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102135486A (en) * | 2010-12-22 | 2011-07-27 | 中国科学院山西煤炭化学研究所 | Method for quickly detecting concentration of polyacrylonitrile-based free radical coagulation bath |
| CN102879356A (en) * | 2012-09-28 | 2013-01-16 | 邢台钢铁线材精制有限责任公司 | Method for measuring concentration of passivation tank liquid for galvanization |
| CN103674894A (en) * | 2013-12-30 | 2014-03-26 | 安徽皖维集团有限责任公司 | Method for detecting concentration of polyvinyl alcohol solution in production of polyvinyl-alcohol optical film by utilizing refractometer |
| CN106770915A (en) * | 2016-12-14 | 2017-05-31 | 威海拓展纤维有限公司 | The method of quick test carbon fiber electrolytic liquid concentration |
| CN109975243A (en) * | 2019-04-04 | 2019-07-05 | 山西钢科碳材料有限公司 | The quickly method of measurement polyacrylonitrile solid content |
| CN111551425A (en) * | 2020-05-28 | 2020-08-18 | 山西钢科碳材料有限公司 | Method for determining content of dimethyl sulfoxide in sample in purification process |
| CN113311112A (en) * | 2021-05-22 | 2021-08-27 | 威海市计量所 | Carbon fiber precursor coagulation bath production field simulation device, platform and method device |
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| CN101013089A (en) * | 2007-02-02 | 2007-08-08 | 威海拓展纤维有限公司 | On-line detecting method of stiffening agent concentration during carbon fibre production process |
| CN101017136A (en) * | 2007-02-02 | 2007-08-15 | 威海拓展纤维有限公司 | Online testing method for oil solution concentration of polyacrylonitile production used in carbon fiber |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102135486A (en) * | 2010-12-22 | 2011-07-27 | 中国科学院山西煤炭化学研究所 | Method for quickly detecting concentration of polyacrylonitrile-based free radical coagulation bath |
| CN102879356A (en) * | 2012-09-28 | 2013-01-16 | 邢台钢铁线材精制有限责任公司 | Method for measuring concentration of passivation tank liquid for galvanization |
| CN103674894A (en) * | 2013-12-30 | 2014-03-26 | 安徽皖维集团有限责任公司 | Method for detecting concentration of polyvinyl alcohol solution in production of polyvinyl-alcohol optical film by utilizing refractometer |
| CN106770915A (en) * | 2016-12-14 | 2017-05-31 | 威海拓展纤维有限公司 | The method of quick test carbon fiber electrolytic liquid concentration |
| CN109975243A (en) * | 2019-04-04 | 2019-07-05 | 山西钢科碳材料有限公司 | The quickly method of measurement polyacrylonitrile solid content |
| CN111551425A (en) * | 2020-05-28 | 2020-08-18 | 山西钢科碳材料有限公司 | Method for determining content of dimethyl sulfoxide in sample in purification process |
| CN113311112A (en) * | 2021-05-22 | 2021-08-27 | 威海市计量所 | Carbon fiber precursor coagulation bath production field simulation device, platform and method device |
| CN113311112B (en) * | 2021-05-22 | 2024-03-29 | 威海市计量所 | Carbon fiber precursor coagulation bath production site simulation device, platform and method device |
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Open date: 20101027 |