CN103558163A - Detection method for dye system polarizer dyeing solution composition concentration change - Google Patents
Detection method for dye system polarizer dyeing solution composition concentration change Download PDFInfo
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- CN103558163A CN103558163A CN201310235555.XA CN201310235555A CN103558163A CN 103558163 A CN103558163 A CN 103558163A CN 201310235555 A CN201310235555 A CN 201310235555A CN 103558163 A CN103558163 A CN 103558163A
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Abstract
The present invention discloses a detection method for dye system polarizer dyeing solution composition concentration change. The method comprises: preparing standard solutions with different dye ratios and a unknown sample hue curve solution, detecting optical properties such as hue and absorbance of the solution, determining the dye ratio of the unknown sample according to the hue coefficients of the standard solution and the unknown sample solution, and calculating the absorption coefficient and the concentration of the unknown sample. According to the present invention, the hue coefficient is adopted to determine the dyeing solution ratio of the unknown sample, the absorption coefficient of the unknown sample is calculated, the total concentration is calculated, and concentrations of various dyes are obtained according to the dyeing solution ratio of the unknown sample so as to effectively monitor the dyeing solution concentration change; and the detection method has significant advantages of accuracy, convenience, cost saving, rapidness and the like, can be applied in the polarizer industry and textile industry, and can further be widely used in various dyeing industries.
Description
Technical field
The present invention relates to a kind of dyestuff is the detection method of polaroid dyeing liquor constituent concentration change, the detection method of the dyeing liquor that particularly relevant two dye solution forms, online test method when its method can be used as continuous production, the concentration change of immediately monitoring constituent, determine the addition of each constituent, guarantee to produce continuously the optical stability of polaroid.
Background technology
Along with display device applications scope is more and more extensive, more and more use under rugged environment (as high temperature, hot and humid), therefore need to develop and have excellent durability polaroid.Dyestuff is the wear properties that light polarizing film has rich color and better high temperature resistant, wet-heat resisting, can be used for, in the outdoor dedicated display such as higher vehicle-mounted, the aircraft of environmental requirement or square, therefore having obtained paying close attention to widely.With dichroic dye, replace iodine/potassium iodide to produce high durable polaroid, but only with a kind of homogencous dyes, cannot obtain suitable polaroid form and aspect, conventionally by two to four kinds of dyestuff mixing preparations, go out applicable dyestuff.The dyeing liquor mixing for multiple dyestuff in process of production, dyes in film because dyestuff adsorbs gradually, and the concentration in dyeing liquor constantly reduces.And the dyeing rate of each dyestuff is different, cause after polaroid produces a period of time continuously, the ratio of the various dyestuffs in dyeing liquor is different when just having started, thus it is stable to have affected the optics form and aspect of polaroid.Therefore, need the ratio of on-line monitoring dyeing liquor, the variation of concentration, add timely dyestuff.It is an important directions of staining technique progress that the dye strength of on-line monitoring dyeing course changes.But stin of thickness on-line monitoring technique is at present also in the starting stage in the world, and application is aborning blank substantially, also have a lot of technical matterss to need to solve.Its subject matter records the dye strength in dyeing liquor accurately and rapidly in being on a large scale, especially measure each dye strength that mixes dye liquor.
Conventional spectrophotometry maximum absorption wavelength is at a distance of the mixing dye liquor concentration of larger dyestuff, and error is less.When two kinds of dye colours approach, absorption spectrum is overlapping serious, or the relative concentration of one of them dyestuff is when other components are very little, and error at measurment is larger.
At present, the assay method of dye strength mainly contains spectrophotometric method, liquid phase chromatography, fluorescence spectrophotometry, derivative spectrophotometry, K ratio method etc.Liquid phase chromatography, when measuring mixed dye concentration, need to be carried out separation to sample, measures consuming time longlyer, is mainly used in off-line analysis; Fluorescence spectrophotometry requires component to be measured to have certain fluorescence quantum yield, and the Coexisting component such as solvent is very large to the fluorescence peak position of dye liquor and intensity effect, general only for the mensuration of extremely low concentration; And spectrophotometric rule can be from dyeing liquor continuously or timing sampling, by the variation of spectrophotometric determination dyeing liquor absorbance, can realize the Real-Time Monitoring to dyeing course, have highly sensitive, selectivity better, measure fast, instrument price is lower, use the features such as wide, but for the dyeing liquor computing method more complicated of mixed dye.Yellow rainbow, Zhang Zhi are refined, Jin Fujiang measures in mixing each concentration of component of dye liquor > > and points out in < < determination method of improved while, adopt absorbance log-wavelength-concentration model method to measure the concentration of mixed dye liquid.Wang Zhi brightness < < utilizes the Primary Study > > of three kinds of coloring agent compositions in SIMULTANEOUS DETERMINATION mixed dye to adopt partial least-squares regression method to carry out the dye strength of three kinds of mixed dye liquid of quantitative test.But its method has been used in independent variable matrix and dependent variable matrix and has been extracted partially minimum binary, resolves by visible spectrum, adopt inner validation-cross to extract main cause subnumber, set up and measure the new method that three components are mixed dye liquor concentration simultaneously.These methods are calculated more complicated, are not suitable for industrial use, higher to Manufacturing Worker's competency profiling, and producers have certain difficulty to operation, grasp.
In order to overcome the problems referred to above, the present invention proposes a kind of characteristic parameter of dyestuff---form and aspect coefficient, by form and aspect coefficient, not only can detect dye strength and change, can also judge the model of dyestuff, the ratio of dyestuff etc., also can be used as the method for inspection foundation of polaroid industry dyestuff charging.The present invention is combined dyestuff form and aspect coefficient with utilizing the additive property principle of polycomponent absorbance, can facilitate, the constituent concentration change of analyzing and testing dyeing liquor simply, determine the interpolation speed of dyeing rate, consumption and the various amount of dye of each dyestuff, can realize the real-time monitoring to dyeing course, especially the stin of thickness that is applied to two component dyestuffs changes and detects, for the universal and development of dyeing on-line monitoring technique provides reference.The present invention can also be for judging the model of dyestuff, as dyestuff starting material receiving inspection method.The remarkable advantages such as it is accurate, simple and easy, cost-saving, quick that the present invention has, this technology can obtain compared with widespread use.
Summary of the invention
The invention discloses a kind of characteristic parameter of dyestuff, a kind of dyestuff its solution form and aspect a, b under variable concentrations have certain relation, and meet the linear relationship of linear function, and this linear relationship is called " form and aspect curve " in the present invention.The solution of different dyes, the dye solution of different proportion have different form and aspect curves, have different form and aspect coefficients, so form and aspect coefficient is a kind of special parameter of dye solution.Therefore can judge by form and aspect coefficient the ratio of dyeing liquor, the additive property principle of recycling polycomponent absorbance calculates the actual concentrations of each component dyestuff.
The object of the invention is to disclose a kind of detection method of dyestuff polaroid dyeing liquor constituent concentration change, by in conjunction with absorbance-concentration curve and dyestuff form and aspect curve, detect the constituent concentration change of two component dyeing liquid, effectively monitor stin of thickness and change, determine the interpolation speed of dyeing rate, consumption and the various amount of dye of each dyestuff.Understand dyestuff under varying environment, in different process situation simultaneously, the dyeing rate of dyestuff, thus select optimum dyeing.
Another object of the present invention is, proposes a kind of characteristic-form and aspect curve of dyestuff, and form and aspect coefficient is as the special parameter of dyestuff, not only can be used as dye strength and changes and detect, can also be as the method foundation of dyestuff charging inspection.
In order to achieve the above object, the detection method that a kind of dyestuff is polaroid dyeing liquor constituent concentration change.The method comprises the steps:
(1) preparation mark liquid, the standard solution of preparation different dyes ratio mixed dye liquid;
(2) prepare unknown sample form and aspect curve solution;
(3) solution optical detecting, measures solution optical property, as absorbance, form and aspect (a, b);
(4) calculate dyestuff ratio, by the form and aspect coefficient of standard solution and unknown sample solution, determine the dyestuff ratio of unknown sample.By measuring the solution form and aspect optics (a, b) of dye solution under variable concentrations, by formula (1), carry out curve fitting, slope is form and aspect coefficient f, selects M, two dye solutions of N, and their dyestuff ratio is respectively m, n, and form and aspect coefficient is respectively f
1, f
2, according to formula (2) calculate again unknown sample be by M, two dye solutions of N in proportion x mix, according to formula (3), calculate dye solution proportion of composing y;
b=f×a?
In formula (1): a, b represent the characteristic of polaroid color, adopt International Commission on Illumination (CIE) 1976 L a b chromaticity coordinate systems.A represents form and aspect, represents red green direction, and positive interval scale is red, and negative interval scale is green; B represents chroma, represents champac direction, and b is that timing is yellow, and negative interval scale is blue.F is matched curve coefficient between the form and aspect b of solution under variable concentrations and a, and the present invention is called " form and aspect coefficient ", and every kind of dyestuff has specific form and aspect coefficient;
(5) calculate dye strength.According to Lambert-Beer's law A=k * [C], utilize the typical curve of different proportion to calculate the total concentration of unknown sample solution, then according to dyestuff ratio, calculate the concentration of various dyestuffs.By measuring the absorbance of solution under variable concentrations, carry out absorbance A-concentration [C] and carry out curve fitting, slope is absorptivity k.Select two M, N dye solution, their absorptivitys are respectively k
1, k
2.According to formula (4), calculate the absorptivity k of unknown sample
3, absorbance A-the concentration of unknown sample dye solution [C] typical curve formula is A
3=k
3* [C], can calculate the total concentration of unknown dye solution simply.According to the proportional y of the dye set of unknown sample, calculate respectively the concentration of each dyestuff, i.e. the variation of known dye strength again;
k3=k1÷(x+1)+k2×x÷(x+1)
In formula (4): k is the coefficient of dyestuff absorbance-concentration [C] standard working curve, i.e. absorptivity, every kind of dyestuff has specific absorptivity.[C] represents solution concentration.
The standard solution absorbance of described step (1) variable concentrations between 10～80%, preferably 15～65%.
The unknown sample form and aspect of the preparation curve solution of described step (2), refers to the solution that unknown sample is mixed with to variable concentrations, and the absorbance of solution is 10～80%, preferably between 15～65%.
The solution optical detecting of described step (3), refers to that solution detects absorbance or transmitance, form and aspect a, b optical property in instrument, and these instruments can be spectrophotometer, colour difference meter, colorimeter, preferably spectrophotometer.
The characteristic parameter that the dyestuff form and aspect coefficient of described step (4) is a kind of dyestuff, refers to that form and aspect optics (a, b) carries out curve fitting, and the curvilinear function of its matching is linear function.The form and aspect coefficient f of unknown sample
3, should meet f
2<f
3<f
1condition, M, N dye solution ratio be at a distance of fewer, the f calculating
3more accurate.
The A of described step (5)
3=k
3* [C], its A
3between 24～50%, preferably 35%～45%.
The present invention judges the ratio y of unknown sample dye solution by form and aspect coefficient, then calculates the absorbance coefficient k of this unknown sample
3then calculate total concentration, finally according to the dye solution ratio of unknown sample, draw the concentration of each dyestuff, known each dye strength changes, effectively monitoring stin of thickness changes, thereby determine the speed of adding of dyeing rate, consumption and the various amount of dye of each dyestuff, can guarantee the stable of production, improve the quality of product.The present invention can also be as the foundation of dyestuff receiving inspection method.The remarkable advantages such as it is accurate, easy to operate, cost-saving, quick that the present invention has, Manufacturing Worker can grasp rapidly, both can be applicable in polaroid industry, can be applicable to again textile industry, can also be widely used in each large field industry of dyeing.
Embodiment
embodiment 1
A kind of dyestuff of the present invention is the detection method of polaroid dyeing liquor constituent concentration change, below just the present invention be elaborated.Following explanation only includes crucial emphasis step to the description of step, does not comprise whole complete process.The existing skill that the present invention continues to use, only quotes and does not elaborate, and is mainly convenient to elaboration of the present invention.
A kind of dyestuff of the present invention is the detection method of polaroid dyeing liquor constituent concentration change, in conjunction with preferred embodiment 1 of the present invention, comprises the steps: now
(1) preparation mark liquid, prepares respectively dyestuff 1 and dyestuff 2 ratios and is 1.275,1.367 M, N dye solution standard solution;
(2) prepare unknown sample form and aspect curve solution, get unknown sample dyeing liquor 1#, 2# in production run, two samples are separated by 1 hour, according to the method for standard solution, prepare form and aspect curve solution;
(3) solution optical detecting, by spectrophotometric determination solution absorbance, form and aspect (a, b).From table 1, the form and aspect coefficient f of M dye solution
1form and aspect coefficient f for-1.0424, N
2for-1.0563, the form and aspect coefficient f of unknown sample dyeing liquor 1#
3for-1.0557, the form and aspect coefficient f of unknown sample dyeing liquor 2#
4for-1.0481.The absorptivity of M is that the absorptivity of 5767.6, N is 5822.9;
Table 1 A-[C] typical curve and form and aspect parameter of curve
(4) calculate dyestuff ratio, according to formula (2), calculate the x of unknown sample dyeing liquor 1#
3=(f
3-f
2) ÷ (f
1-f
3)=0.045, so the dyeing liquor 1# ratio of unknown sample is by formula (3) calculating, y
3=m * x ÷ (x+1)+n ÷ (x+1)=1.284; Same method, calculates the x of unknown sample dyeing liquor 2#
4be 1.206, y
4be 1.329;
(5) calculate dye strength, table 2 result of calculation is visible, calculates the absorptivity of unknown sample dyeing liquor 1#, k according to formula (4)
3=k
1÷ (x+1)+k
2* x ÷ (x+1)=5769.99, while method, calculates the absorptivity k that calculates unknown sample dyeing liquor 2#
4be 5797.84.Unknown sample dyeing liquor 1# total concentration is 0.113%, and the concentration of dyestuff 1 is 0.063%, and the concentration 2 of dyestuff 2 is 0.049%.Unknown sample dyeing liquor 2# total concentration is 0.106%, and the concentration of dyestuff 1 is 0.061%, and the concentration 2 of dyestuff 2 is 0.046%.
Table 2 result of calculation
The concentration change of being separated by one hour sample time from unknown sample dyeing liquor 1#, 2# can be judged, and dyestuff 1 concentration reduces 0.002%, and dyestuff 2 concentration reduce 0.003%.As long as know that the volume of staining trough makes the additional amount of 1,2 minutes other consumptions of known dyestuff and dye solution, guarantee that quantity-produced product is stable.
reference examples 1
A kind of dyestuff of the present invention is the detection method of polaroid dyeing liquor constituent concentration change., in conjunction with the inventive method step, carry out the known sample of reference examples and detect now, the error of check the inventive method, verifies its accuracy.Comprise the steps:
(1) preparation mark liquid, prepares respectively dyestuff 1 and dyestuff 2 ratios and is 1.58,1.77 M, N dye solution standard solution;
(2) prepare unknown sample form and aspect curve solution, the form and aspect curve solution that preparation dyestuff 1 and dyestuff 2 ratios are 1.66;
(3) solution optical detecting, by spectrophotometric determination solution absorbance, form and aspect (a, b).As shown in Table 3, the form and aspect coefficient f of M dye solution
1form and aspect coefficient f for-1.0611, N
2for-1.069, the form and aspect coefficient f of known sample
3for-1.0638.The absorptivity of M is that the absorptivity of 5547.4, N is 5685.3, and the absorptivity of known sample is 5645.6;
Table 3 A-[C] typical curve and form and aspect curve
(4) calculate dyestuff ratio, according to formula (2), calculate x=(f
3-f
2) ÷ (f
1-f
3)=1.926, so the dyestuff ratio of unknown sample is by formula (3) calculating, y=m * x ÷ (x+1)+n ÷ (x+1)=1.65;
(5) calculate dye strength, according to formula (4), calculate the absorptivity of unknown sample, K3=K1/ (x+1)+K2 * x/ (x+1)=5547.4/ (1.926+1)+5685.3 * 1.926/ (1.926+1)=5638.17.Select other form and aspect curve solution, total concentration is 0.0078%, and the concentration of dyestuff 1 is 0.0049%, and the concentration 2 of dyestuff 2 is 0.003%.
The relative error of table 4 detection method of the present invention
As seen from Table 4, detection method relative error of the present invention is in relative error 2%～5% scope of spectrophotometric method, consistent with the relative error of spectrophotometric method.So detection method accuracy of the present invention is consistent with spectrophotometric method, without adding in addition new instrument, operation is simple, convenient again, lower to operative employee's requirement, can be widely used in each large fields such as polaroid manufacturing industry, dyestuff textile industry.
Above-described embodiment is only possible embodiments of the present invention, not in order to limit the scope of the invention, such as be familiar with the personage of this skill, use the equivalence that instructions of the present invention and claim scope are done to change, within ought to being included in the scope of present patent application.
Claims (6)
1. dyestuff is a detection method for polaroid dyeing liquor constituent concentration change, it is characterized in that comprising the steps:
(1) preparation mark liquid, the standard solution preparation of preparation different dyes ratio dye solution;
(2) prepare unknown sample form and aspect curve solution;
(3) solution optical detecting, measures solution absorbance, form and aspect (a, b);
(4) calculate dyestuff ratio, by the form and aspect coefficient of standard solution and unknown sample solution, determine the dyestuff ratio of unknown sample;
(5) calculate dye strength, according to Lambert-Beer's law A=K * [C], utilize the typical curve of different proportion to calculate the total concentration of unknown sample solution, then according to dyestuff ratio, calculate the concentration of various dyestuffs.
2. method according to claim 1, is characterized in that between the standard solution absorbance 10～80% of step (1) variable concentrations, preferably 15～65%.
3. method according to claim 1, is characterized in that step (2) prepares unknown sample form and aspect curve solution, refers to the solution that unknown sample is mixed with to variable concentrations, and the absorbance 10～80% of solution, preferably between 15～65%.
4. method according to claim 1, it is characterized in that step (3) solution optical detecting refers to that solution detects absorbance or transmitance, form and aspect a, b in instrument, these instruments can be spectrophotometer, colour difference meter, colorimeter, preferably spectrophotometer.
5. method according to claim 1, is characterized in that a kind of characteristic parameter that step (4) dyestuff form and aspect coefficient is dyestuff, and the form and aspect optics (a, b) by the dye solution under curve variable concentrations, obtains b=f * a linear function.
6. method according to claim 1, is characterized in that absorbance that step (5) calculates unknown sample concentration solution is between 24～50%, preferably 35%～45%.
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Cited By (4)
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| CN104614319A (en) * | 2014-12-22 | 2015-05-13 | 福建宇邦纺织科技有限公司 | A method of digitized analysis of compatibility of a dye composition by adoption of a spectrometer |
| CN105300904A (en) * | 2015-11-04 | 2016-02-03 | 深圳市盛波光电科技有限公司 | Dye concentration detection method in dye type polaroid production process |
| CN108680521A (en) * | 2018-05-18 | 2018-10-19 | 黎明职业大学 | A kind of component analyzing method and color monitoring method |
| CN110987845A (en) * | 2019-11-26 | 2020-04-10 | 武汉纺织大学 | Real-time detection method for dye concentration in single-component and double-component dye solutions |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104614319A (en) * | 2014-12-22 | 2015-05-13 | 福建宇邦纺织科技有限公司 | A method of digitized analysis of compatibility of a dye composition by adoption of a spectrometer |
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| CN108680521A (en) * | 2018-05-18 | 2018-10-19 | 黎明职业大学 | A kind of component analyzing method and color monitoring method |
| CN110987845A (en) * | 2019-11-26 | 2020-04-10 | 武汉纺织大学 | Real-time detection method for dye concentration in single-component and double-component dye solutions |
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