CN101004381A - Method for detecting concentration of oil solution in producing polyacrylonitrile raw yarn in use for carbon fiber - Google Patents
Method for detecting concentration of oil solution in producing polyacrylonitrile raw yarn in use for carbon fiber Download PDFInfo
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Abstract
A method for detecting concentration of oiling agent in production of polyacry / onitrile raw filament being used to prepare carbon fiber includes obtaining concentration and refractive power of oiling agent, optimizing linear equation, sampling, measuring refractive power and converting measured refractive power to be concentration.
Description
Technical field
The invention belongs to measuring technique, relate to improvement oil concentration detection method in the polyacrylonitrile fibril for carbon fiber production run.
Background technology
PAN-based carbon fiber has characteristics such as high specific strength, high ratio modulus, high temperature resistant, corrosion-resistant, creep resistant, stability are strong, and at Aero-Space, mechano-electronic, chemical building material, every field such as energy traffic all have boundless application.PAN-based carbon fiber is produced and is comprised polyacrylonitrile fibril production and two big links of precursor carbonization, and wherein precursor production is key link, and the quality of precursor and quality stability have decisive influence to the quality and the quality stability of final carbon fiber product.Polyacrylonitrile fibril production comprises polymerization, deaeration, takes off list, spinning, wash, oil, multiple tracks technology such as drawing-off.Oiling process is the important ring during polyacrylonitrile fibril is produced, and no matter is wet spinning or dry-jet wet-spinning, and the operation that oils all directly influences the quality of PAN precursor, also final carbon fiber character is had significant impact.It is not good enough not oil or oil, and can cause between the monofilament sticking chain, cause the carbon fiber pulling strengrth descend [Zhang Yinzhi, He Fu, Wang Maozhang, PAN high-performance carbon fibre precursor general situation of development. synthetic fiber industry, 1993,16 (2): 54～57].Good heat resistance, good, the wear-resisting wiping of spreadability, 200 ℃ of left and right sides resistances to oxidation, the volatile product of high temperature are adopted in the selection of oil agent kind usually.Finish at the adhesion amount on the former silk fiber usually between 0.2～2.0% (massfraction), more or less according to finish kind and experimental result and decide.The finish quantity not sufficient can not form the oil film of lubricate at fiber surface, can the damage monofilament surface in the subsequent technique; The finish amount is too much, is difficult for volatilization in the carbonization process fully, influences the pulling strengrth and the breaking elongation of carbon fiber.Therefore the concentration of controlling finish in the finish work pool guarantees that the finish adhesion amount on the polyacrylonitrile fibril becomes the key link of oiling process in the polyacrylonitrile fibril production run near the optimum value that oiling process is determined in stable scope.The concentration of controlling finish in the finish work pool must accurately be measured the concentration of work pool in stable scope.Traditional chemical method is determined oil content in the finish work pool, a plurality of steps such as generally include sampling, volatilization, evaporate to dryness, weigh, and length consuming time, measuring error is big, is unfavorable for the process control of oil concentration in the polyacrylonitrile fibril production run.
Summary of the invention
The objective of the invention is to: a kind of method that fast, accurately detects oil concentration in the polyacrylonitrile fibril for carbon fiber production run is provided.To overcome the shortcoming of traditional chemical method, improve the dynamic and the accuracy of oil concentration control in the polyacrylonitrile fibril production run.
Technical scheme of the present invention is: the detection method of oil concentration during a kind of polyacrylonitrile fibril for carbon fiber is produced is characterized in that use the method for measuring finish refraction index or pol to detect its concentration, it is as follows to detect step:
1, obtains the typical curve of oil concentration and refraction index or pol;
1.1, the agent concentration titer makes up oil; Adopt the finish titer of raw material preparation variable concentrations identical in the polyacrylonitrile fibril for carbon fiber production; If the round values of measured oil agent concentration value is α %, the quantity of the concentration standard liquid of then being prepared is at least 5, 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, and the spacing of two adjacent concentration of standard solution numerical value is 0.1* α %～0.5* α %; The value X of the agent concentration titer that makes up oil
0Expression;
1.2, the refraction index or the pol value Y of bioassay standard liquid
0Use handheld refractometer or Abbe refractometer or digital refractometer to measure the refraction index or the pol value Y of oil concentration titer
0To measure numerical value input computing machine;
1.3, the standard straight-line equation of match oil concentration and refraction index or pol; Adopt least square method to carry out linear fit by interpolation, obtain standard straight-line equation, standard deviation S D and the degree of correlation RD of oil concentration and refraction index or pol, straight-line equation is:
y＝ax+b [1]
In the formula, y is a refraction index, and x is an oil concentration;
2, optimize straight-line equation; At first, the standard deviation S D and the degree of correlation RD of checking straight-line equation; The refraction index of the titer that step 1.1.2 is measured or pol be substitution formula [1] respectively, calculates the calculated value X under this oil concentration, according to X
0And X, calculate standard deviation S D and degree of correlation RD, if standard deviation S D is not more than 1, degree of correlation RD is greater than 0.9 simultaneously, this straight-line equation can directly use; Otherwise repeating step 1.1 increases the quantity of concentration standard liquid, obtain straight-line equation again after, carry out straight-line equation optimization according to this step again, till above-mentioned requirements; Deposit the optimization straight-line equation that obtains in computing machine;
3, sampling; From production line oil agent work pool, extract the sample of tested finish;
4, measure refraction index or pol and be scaled concentration; Use handheld refractometer or Abbe refractometer or digital refractometer to measure the refraction index or the pol value Y of finish sample; To measure numerical value input computing machine, be converted into concentration value X output.
Advantage of the present invention is: the present invention adopts mensuration finish refraction index or pol to converse the method for concentration, can determine the concentration of finish rapidly and accurately, the concentration that helps controlling finish in the finish work pool guarantees that finish adhesion amount on the polyacrylonitrile fibril is near the optimum value that oiling process is determined in stable scope.Method of testing of the present invention fast, accurately, and is suitable for large-scale promotion.
Embodiment
Below the present invention is described in further details.Detection method of the present invention is characterized in that, uses the method for measuring finish refraction index or pol to detect its concentration, and it is as follows to detect step:
1, obtains the typical curve of oil concentration and refraction index or pol;
1.1, the agent concentration titer makes up oil; Adopt the finish titer of raw material preparation variable concentrations identical in the polyacrylonitrile fibril for carbon fiber production; If the round values of measured oil agent concentration value is α %, the quantity of the concentration standard liquid of then being prepared is at least 5, 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, and the spacing of two adjacent concentration of standard solution numerical value is 0.1* α %～0.5* α %; The value X of the agent concentration titer that makes up oil
0Expression.
1.2, the refraction index or the pol value Y of bioassay standard liquid
0Use handheld refractometer or Abbe refractometer or digital refractometer to measure the refraction index or the pol value Y of oil concentration titer
0To measure numerical value input computing machine.Commercially available finished product is counted in employed handheld refractometer or Abbe refractometer or digital refraction.
1.3, the standard straight-line equation of match oil concentration and refraction index or pol; Adopt least square method to carry out linear fit by interpolation, obtain standard straight-line equation, standard deviation S D and the degree of correlation RD of oil concentration and refraction index or pol, straight-line equation is:
y＝ax+b [1]
In the formula, y is a refraction index, and x is an oil concentration.
2, optimize straight-line equation; At first, the standard deviation S D and the degree of correlation RD of checking straight-line equation; The refraction index of the titer that step 1.1.2 is measured or pol be substitution formula [1] respectively, calculates the calculated value X under this oil concentration, according to X
0And X, calculate standard deviation S D and degree of correlation RD, if standard deviation S D is not more than 1, degree of correlation RD is greater than 0.9 simultaneously, this straight-line equation can directly use; Otherwise repeating step 1.1 increases the quantity of concentration standard liquid, obtain straight-line equation again after, carry out straight-line equation optimization according to this step again, till above-mentioned requirements; Deposit the optimization straight-line equation that obtains in computing machine.
3, sampling; From production line oil agent work pool, extract the sample of tested finish.
4, measure refraction index or pol and be scaled concentration; Use handheld refractometer or Abbe refractometer or digital refractometer to measure the refraction index or the pol value Y of finish sample; To measure numerical value input computing machine, be converted into concentration value X output.
Embodiment.
Example 1, the oil concentration fast detecting of certain trade mark
1, obtains the typical curve of oil concentration and refraction index;
1.1, the agent concentration titer makes up oil; If the round values of measured oil agent concentration value is α %, the quantity of the concentration standard liquid of then being prepared is at least 5, 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, and the spacing of two adjacent concentration of standard solution numerical value is 0.1* α %～0.5* α %; Select 6 points in this example for use, particular content sees Table 1.
The concentration value of table 1 concentration standard liquid
| Sample number into spectrum | Concentration (%) |
| 1 | 0.09728 |
| 2 | 0.20429 |
| 3 | 0.30372 |
| 4 | 0.39584 |
| 5 | 0.50544 |
| 6 | 1.03123 |
1.2, the refraction index of bioassay standard liquid; Use digital refractometer to measure the refraction index of oil concentration titer; To measure numerical value input computing machine.Measurement result sees Table 2.
Table 2 refraction index measurement result
| Sample number into spectrum | Concentration (%) | Refraction index |
| 1 | 0.09728 | 1.33201 |
| 2 | 0.20429 | 1.33212 |
| 3 | 0.30372 | 1.33222 |
| 4 | 0.39584 | 1.332 33 |
| 5 | 0.50544 | 1.33242 |
| 6 | 1.03123 | 1.33296 |
1.3, the standard straight-line equation of match oil concentration and refraction index; Adopt least square method to carry out linear fit by interpolation, the standard straight-line equation that obtains oil concentration and refraction index is:
y＝0.00102x+1.33191 [1]
Y is a refraction index in the formula, and x is an oil concentration.
2, optimize straight-line equation; At first, the standard deviation S D and the degree of correlation RD of checking straight-line equation; The refraction index of the titer that step 1.1.2 is measured is substitution formula [1] respectively, calculates the calculated value X under this oil concentration, according to X
0And X, through calculating, the character of straight-line equation y=0.00102x+1.33191 is as follows: degree of correlation RD=0.9998, standard deviation S D=8.2E-6 meets accuracy requirement, can directly use.
3, sampling; From production line oil agent work pool, extract the sample of tested finish.
4, measure refraction index or pol and be scaled concentration; Use has the refraction index Y of the digital refractive index equipment mensuration finish sample of computing function; Be converted into concentration value X output, following table 3 is one group of measurement result.Measure and can finish with interior in 2 minutes, method fast, efficient.
Table 3 measurement result for example
| Concentration X (%) | Refraction index Y |
| 0.06287 | 1.33198 |
| 0.12186 | 1.33204 |
| 0.18084 | 1.3321 |
| 0.23983 | 1.33216 |
| 0.29882 | 1.33222 |
| 0.3578 | 1.33228 |
| 0.47578 | 1.3324 |
| 0.59375 | 1.33252 |
| 0.65273 | 1.33258 |
| 0.71172 | 1.33264 |
| 0.77071 | 1.3327 |
| 0.88868 | 1.33282 |
| 0.94767 | 1.33288 |
| 1.00665 | 1.33294 |
| 1.06564 | 1.3330 |
Example 2, the oil concentration fast detecting of certain trade mark
1, obtains the typical curve of oil concentration and pol;
1.1, the agent concentration titer makes up oil; Adopt the finish titer of raw material preparation variable concentrations identical in the polyacrylonitrile fibril for carbon fiber production; If the round values of measured oil agent concentration value is α %, the quantity of the concentration standard liquid of then being prepared is at least 5, 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, and the spacing of two adjacent concentration of standard solution numerical value is 0.1* α %～0.5* α %; Select 11 points in this example for use, particular content sees Table 4.
The concentration value of table 4 concentration standard liquid
| Sample number into spectrum | Concentration (%) |
| 1 | 14.0004 |
| 2 | 15.9785 |
| 3 | 18.001 |
| 4 | 19.99768 |
| 5 | 22.0533 |
| 6 | 24.0087 |
| 7 | 25.9702 |
| 8 | 27.9663 |
| 9 | 29.89119 |
| 10 | 31.9851 |
| 11 | 33.9714 |
1.2, the pol value of bioassay standard liquid; Use digital saccharometer to measure the pol value of oil concentration titer; To measure numerical value input computing machine.Measurement result sees Table 5.
Table 5 refraction index measurement result
| Sample number into spectrum | Concentration value (%) | The pol value |
| 1 | 14.0004 | 8.59 |
| 2 | 15.9785 | 9.85 |
| 3 | 18.0010 | 10.99 |
| 4 | 19.9977 | 12.24 |
| 5 | 22.0533 | 13.36 |
| 6 | 24.0087 | 14.45 |
| 7 | 25.9702 | 15.56 |
| 8 | 27.9663 | 16.74 |
| 9 | 29.8912 | 17.73 |
| 10 | 31.9851 | 19.01 |
| 11 | 33.9714 | 20.01 |
1.3, the standard straight-line equation of match oil concentration and refraction index; Adopt least square method to carry out linear fit by interpolation, the standard straight-line equation that obtains oil concentration and refraction index is:
y＝0.57047x+0.72974 [1]
Y is the pol value in the formula, and x is an oil concentration.
2, optimize straight-line equation; At first, the standard deviation S D and the degree of correlation RD of checking straight-line equation; The pol value of the titer that step 1.1.2 is measured is substitution formula [1] respectively, calculates the calculated value X under this oil concentration, according to X
0And X, through calculating, the character of straight-line equation y=0.57047x+0.72974 is as follows: degree of correlation RD=0.9998, standard deviation S D=0.07 meets the production line accuracy requirement, can directly use.
3, sampling; From production line oil agent work pool, extract the sample of tested finish.
4, measure refraction index or pol and be scaled concentration; Use has the pol value Y of the digital saccharometer mensuration finish sample of computing function; Be converted into concentration value X output, following table 6 is one group of measurement result.Measure and can finish with interior in 2 minutes, this method fast, efficient.
Table 6 measurement result for example
| Concentration value (%) | The pol value |
| 12.0033 | 7.57723 |
| 13.26463 | 8.29678 |
| 14.52595 | 9.01632 |
| 15.78728 | 9.73587 |
| 17.04861 | 10.45541 |
| 18.30993 | 11.17496 |
| 19.57126 | 11.8945 |
| 20.83258 | 12.61405 |
| 22.09391 | 13.3336 |
| 23.35524 | 14.05314 |
| 24.61656 | 14.77269 |
| 25.87789 | 15.49223 |
| 27.13922 | 16.21178 |
| 28.40054 | 16.93132 |
| 29.66187 | 17.65087 |
| 30.92319 | 18.37041 |
| 32.18452 | 19.08996 |
| 33.44585 | 19.80951 |
| 34.70717 | 20.52905 |
Example 3, the oil concentration fast detecting of certain trade mark
1, obtains the typical curve of oil concentration and refraction index;
1.1, the agent concentration titer makes up oil; If the round values of measured oil agent concentration value is α %, the quantity of the concentration standard liquid of then being prepared is at least 5, 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, and the spacing of two adjacent concentration of standard solution numerical value is 0.1* α %～0.5* α %; Select 10 points in this example for use, particular content sees Table 7.
The concentration value of table 7 concentration standard liquid
| Sample number into spectrum | Concentration (%) |
| 1 | 9.97392 |
| 2 | 11.988 |
| 3 | 14.0004 |
| 4 | 15.9785 |
| 5 | 18.001 |
| 6 | 19.9977 |
| 7 | 22.0533 |
| 8 | 24.0087 |
| 9 | 25.9702 |
| 10 | 27.9663 |
1.2, the refraction index of bioassay standard liquid; Use digital refractometer to measure the refraction index of oil concentration titer; To measure numerical value input computing machine.Measurement result sees Table 8.
Table 8 refraction index measurement result
| Sample number into spectrum | Concentration (%) | Refraction index |
| 1 | 9.97392 | 1.34095 |
| 2 | 11.988 | 1.34275 |
| 3 | 14.0004 | 1.34452 |
| 4 | 15.9785 | 1.34642 |
| 5 | 18.001 | 1.34818 |
| 6 | 19.9977 | 1.35022 |
| 7 | 22.0533 | 1.35185 |
| 8 | 24.0087 | 1.35357 |
| 9 | 25.9702 | 1.35534 |
| 10 | 27.9663 | 1.35723 |
1.3, the standard straight-line equation of match oil concentration and refraction index; Adopt least square method to carry out linear fit by interpolation, the standard straight-line equation that obtains oil concentration and refraction index is:
y＝9.03533E-4x+1.33194 [1]
Y is a refraction index in the formula, and x is an oil concentration.
2, optimize straight-line equation; At first, the standard deviation S D and the degree of correlation RD of checking straight-line equation; The refraction index of the titer that step 1.1.2 is measured is substitution formula [1] respectively, calculates the calculated value X under this oil concentration, according to X
0And X, through calculating, the character of straight-line equation y=9.03533E-4x+1.33194 is as follows: degree of correlation RD=0.9999, standard deviation S D=8.7E-5 meets accuracy requirement, can directly use.
3, sampling; From production line oil agent work pool, extract the sample of tested finish.
4, measure refraction index and be scaled concentration; Use has the refraction index Y of the digital refractometer mensuration finish sample of computing function; Be converted into concentration value X output, following table 9 is one group of measurement result.Measure and can finish with interior in 2 minutes, this method fast, efficient.
Table 9 measurement result for example
| Concentration X (%) | Refraction index Y |
| 8.17468 | 1.33933 |
| 9.31104 | 1.34035 |
| 10.4474 | 1.34138 |
| 11.58376 | 1.34241 |
| 12.72013 | 1.34343 |
| 13.85649 | 1.34446 |
| 14.99285 | 1.34549 |
| 16.12921 | 1.34651 |
| 17.26557 | 1.34754 |
| 19.53829 | 1.34959 |
| 20.67465 | 1.35062 |
| 21.81101 | 1.35165 |
| 22.94737 | 1.35268 |
| 24.08373 | 1.35370 |
| 25.22009 | 1.35473 |
| 26.35646 | 1.35576 |
| 27.49282 | 1.35678 |
| 28.62918 | 1.35781 |
| 29.76554 | 1.35884 |
Claims (1)
1, the detection method of oil concentration is characterized in that during a kind of polyacrylonitrile fibril for carbon fiber was produced, and used the method for measuring finish refraction index or pol to detect its concentration, and it is as follows to detect step:
1.1, obtain the typical curve of oil concentration and refraction index or pol;
1.1.1, the agent concentration titer makes up oil; Adopt the finish titer of raw material preparation variable concentrations identical in the polyacrylonitrile fibril for carbon fiber production; If the round values of measured oil agent concentration value is α %, the quantity of the concentration standard liquid of then being prepared is at least 5, 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, and the spacing of two adjacent concentration of standard solution numerical value is 0.1* α %～0.5* α %; The value X of the agent concentration titer that makes up oil
0Expression;
1.1.2, the refraction index or the pol value Y of bioassay standard liquid
0Use handheld refractometer or Abbe refractometer or digital refractometer to measure the refraction index or the pol value Y of oil concentration titer
0To measure numerical value input computing machine;
1.1.3, the standard straight-line equation of match oil concentration and refraction index or pol; Adopt least square method to carry out linear fit by interpolation, the standard straight-line equation that obtains oil concentration and refraction index or pol is:
y＝ax+b [1]
In the formula, y is a refraction index, and x is an oil concentration;
1.2, optimize straight-line equation; At first, the standard deviation S D and the degree of correlation RD of checking straight-line equation; The refraction index of the titer that step 1.1.2 is measured or pol be substitution formula [1] respectively, calculates the calculated value X under this oil concentration, according to X
0And X, calculate standard deviation S D and degree of correlation RD, if standard deviation S D is not more than 1, degree of correlation RD is greater than 0.9 simultaneously, this straight-line equation can directly use; Otherwise repeating step 1.1 increases the quantity of concentration standard liquid, obtain straight-line equation again after, carry out straight-line equation optimization according to this step again, till above-mentioned requirements; Deposit the optimization straight-line equation that obtains in computing machine;
1.3, the sampling; From production line oil agent work pool, extract the sample of tested finish;
1.4, measure refraction index or pol and be scaled concentration; Use handheld refractometer or Abbe refractometer or digital refractometer to measure the refraction index or the pol value X of finish sample; To measure numerical value input computing machine, be converted into concentration value Y output.
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|---|---|---|---|
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|---|---|---|---|
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| 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 |
| CN111088541A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | Preparation method of polyacrylonitrile fiber |
| 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 |
| CN112432922A (en) * | 2020-09-03 | 2021-03-02 | 中复神鹰碳纤维有限责任公司 | Method for rapidly detecting concentration of oil agent in production of polyacrylonitrile carbon fiber precursor |
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| CN1272622C (en) * | 1998-04-22 | 2006-08-30 | 株式会社理光 | Double refraction detecting method and device |
| JP2001272390A (en) * | 2000-03-27 | 2001-10-05 | Masayoshi Kobayashi | Method for measuring gas sorption amount and gas diffusion coefficient of polymer material |
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| 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 |
| CN111088541A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | Preparation method of polyacrylonitrile fiber |
| 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 |
| CN112432922A (en) * | 2020-09-03 | 2021-03-02 | 中复神鹰碳纤维有限责任公司 | Method for rapidly detecting concentration of oil agent in production of polyacrylonitrile carbon fiber precursor |
| CN112881338A (en) * | 2021-01-11 | 2021-06-01 | 中国农业科学院油料作物研究所 | Mathematical model of peanut oil refractive index, detection method of high-oleic-acid peanuts and identification instrument |
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