CN112082964A - Rapid detection method for content of cationic copolyester modified monomer - Google Patents
Rapid detection method for content of cationic copolyester modified monomer Download PDFInfo
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- 125000002091 cationic group Chemical group 0.000 title claims abstract description 176
- 229920001634 Copolyester Polymers 0.000 title claims abstract description 95
- 239000000178 monomer Substances 0.000 title claims abstract description 73
- 238000001514 detection method Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000002835 absorbance Methods 0.000 claims abstract description 20
- 238000001179 sorption measurement Methods 0.000 claims abstract description 13
- 238000002798 spectrophotometry method Methods 0.000 claims abstract description 5
- 239000000975 dye Substances 0.000 claims description 151
- 238000004043 dyeing Methods 0.000 claims description 55
- 239000000243 solution Substances 0.000 claims description 39
- 239000002245 particle Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 12
- 238000007865 diluting Methods 0.000 claims description 12
- 238000010790 dilution Methods 0.000 claims description 12
- 239000012895 dilution Substances 0.000 claims description 12
- 238000010521 absorption reaction Methods 0.000 claims description 11
- 239000012224 working solution Substances 0.000 claims description 11
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- 239000001632 sodium acetate Substances 0.000 claims description 9
- 235000017281 sodium acetate Nutrition 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 7
- 239000010413 mother solution Substances 0.000 claims description 7
- 239000011780 sodium chloride Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000012086 standard solution Substances 0.000 claims description 6
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 5
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 5
- 239000012452 mother liquor Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 239000003340 retarding agent Substances 0.000 claims description 5
- 239000011975 tartaric acid Substances 0.000 claims description 5
- 235000002906 tartaric acid Nutrition 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- 238000013329 compounding Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 4
- ZQOMKIOQTCAGCM-UHFFFAOYSA-L [Na+].[Na+].OS(O)(=O)=O.[O-]S([O-])(=O)=O Chemical compound [Na+].[Na+].OS(O)(=O)=O.[O-]S([O-])(=O)=O ZQOMKIOQTCAGCM-UHFFFAOYSA-L 0.000 claims description 2
- 235000011054 acetic acid Nutrition 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 2
- 235000011167 hydrochloric acid Nutrition 0.000 claims description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 2
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- 150000001768 cations Chemical class 0.000 abstract description 2
- 229920006395 saturated elastomer Polymers 0.000 abstract 1
- SYHRPJPCZWZVSR-UHFFFAOYSA-M n-benzyl-4-[(2,4-dimethyl-1,2,4-triazol-4-ium-3-yl)diazenyl]-n-methylaniline;bromide Chemical compound [Br-].C=1C=C(N=NC2=[N+](C=NN2C)C)C=CC=1N(C)CC1=CC=CC=C1 SYHRPJPCZWZVSR-UHFFFAOYSA-M 0.000 description 7
- 229920000728 polyester Polymers 0.000 description 7
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- 238000003760 magnetic stirring Methods 0.000 description 2
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- 229910001220 stainless steel Inorganic materials 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- GGAVKFLPQAQTML-UHFFFAOYSA-N CCOC(=O)C1=CC(C(O)=O)=CC(S(O)(=O)=O)=C1 Chemical compound CCOC(=O)C1=CC(C(O)=O)=CC(S(O)(=O)=O)=C1 GGAVKFLPQAQTML-UHFFFAOYSA-N 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
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- 229920006351 engineering plastic Polymers 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
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- 230000007935 neutral effect Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
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- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
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- 229910052708 sodium Inorganic materials 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
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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
- G01N1/30—Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
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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
- G01N1/38—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
- G01N1/30—Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
- G01N2001/302—Stain compositions
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Abstract
The invention discloses a method for rapidly detecting the content of a cationic copolyester modified monomer, which comprises the steps of adding the cationic copolyester to be detected into a dye solution containing a cationic dye, enabling the modified monomer in the cationic copolyester to adsorb the cationic dye until the cationic dye is saturated, measuring the absorbance of the residual dye solution after the cationic copolyester adsorbs the dye by a spectrophotometry, and determining the concentration of the cationic dye in the residual dye solution after adsorption, thereby obtaining the content of the cationic copolyester modified monomer. The method has the advantages of strong operability, high detection result precision and good repeatability, and can meet the requirement of accurate detection of cation modified monomers with different contents.
Description
Technical Field
The invention relates to a method for rapidly detecting the content of a cationic copolyester modified monomer, belonging to the field of quality detection and analysis of polyester chips.
Background
The PET polyester has high strength, good stability and excellent processing performance, and is widely used in the fields of clothes, bottle flakes, films, engineering plastics and the like, wherein the clothes field accounts for 70 percent. Because the PET polyester has good molecular structure linearity and high crystallinity, and a molecular chain is lack of hydrophilic groups and dyeing groups, the dyeing and printing of products are difficult. The traditional PET polyester dyeing and printing process only adopts disperse dyes, and the dyeing process has high energy consumption and high chroma of dyeing wastewater and has great environmental pollution. The cationic modified copolyester is prepared by introducing a trimonomer (SIPE-sodium bis (ethyl-5-sulfoisophthalate)) and carrying out bulk copolymerization modification, the cationic dyeability of the product is endowed, and the adsorption and diffusion capacity of the dye to fibers is greatly improved due to positive and negative charges formed between the fibers and the dye in the cationic dyeing process, so that the dyeing energy consumption is reduced, the chromaticity of dyeing wastewater is low, and the environmental protection effect is obvious.
The cationic modified polyester dyeing is dyeing base dyeing, the dyeing depth is influenced by the SIPE content of the modified monomer, the higher the SIPE content is, and the deeper the dyeing depth is under the same dyeing condition. The downstream market is based on different application fields, the requirements on the SIPE content of the modified monomer in the product are different, and the content of the cationic modified monomer is increased from the initial 2.4 percent to more than 10 percent along with the continuous expansion of the application fields. The industry carries out qualitative analysis on the cationic modified polyester through dyeing with cationic dye, and can only judge whether the cationic modified polyester contains the cationic modified monomer. In the actual production process, the deviation of the cationic modified monomer in the product is often caused by the faults of metering equipment, manual misoperation and the like, so that the content of the modified monomer in the product needs to be quantitatively analyzed in real time. At present, the quantitative analysis needs to be fitted through a nuclear magnetic resonance spectrogram, but the detection instrument has high cost, long analysis time and low operability in the actual production process.
Disclosure of Invention
Based on the defects of the prior art, the invention aims to provide a method for quickly detecting the content of a cationic copolyester modified monomer so as to timely and quickly guide and service production.
In order to realize the purpose of the invention, the following technical scheme is adopted:
a rapid detection method for the content of a cationic copolyester modified monomer is characterized by comprising the following steps: adding to-be-detected cationic copolyester into dye liquor containing cationic dye with known concentration, adsorbing the cationic dye to saturation by using modified monomers in the cationic copolyester, measuring the absorbance of the residual dye liquor after adsorption by using a spectrophotometry, determining the concentration of the cationic dye in the residual dye liquor after adsorption, determining the adsorption amount of the modified monomers in the cationic copolyester to the cationic dye, and obtaining the content of the modified monomers in the cationic copolyester according to the dyeing saturation value of the modified monomers to the cationic dye.
The dyeing saturation value of the modified monomer to the cationic dye refers to that the cationic dye is adsorbed on a negative charge activation center of the cationic copolyester, when the cationic dye is adsorbed by the modified monomer in the cationic copolyester to reach the saturation value, the concentration of the dye in the copolyester is not increased along with the increase of the concentration of the cationic dye in a dye solution, at the moment, the concentration of the dye adsorbed on the cationic copolyester is the dyeing saturation value, the adsorption line is obviously turned into a horizontal line, and the dyeing saturation value (g dye/100 g cationic copolyester with the known modified monomer content) is represented by the dye amount on each 100g cationic copolyester with the known modified monomer content.
Further, the dye solution containing the cationic dye is obtained by dissolving the cationic dye in deionized water, adding a complex retarding agent, and adjusting the pH value to 3.5-6.0 by using a pH regulator; in the dye solution, the concentration of the cationic dye is 0.5-5 g/L, and the concentration of the compound slow-dyeing agent is 2-5 g/L.
Furthermore, in order to increase the stability and accuracy of the detection result, the compatibility value K of the adopted cationic dye is 3-5. The cationic dye of the present invention is preferably a cationic red X-GRL. FIG. 1 is a graph of dye saturation values for dye liquors of different cationic red X-GRL concentrations for several known cationic copolyesters of modified monomer content.
Further, the compound slow-dyeing agent is prepared by compounding at least two of sodium acetate, sodium chloride, disodium hydrogen sulfate, disodium hydrogen phosphate, sodium dihydrogen phosphate and anhydrous sodium sulfate, and preferably is prepared by compounding sodium acetate and sodium chloride according to the mass ratio of 1-4: 0.5-2. The compound retarding agent can fully inhibit the hydrolysis effect of the high-content modified monomer cationic copolyester section dyeing process on the basis of reducing the dyeing speed and improving the level dyeing rate, and the principle is that in a formed buffer system, an anion component in neutral salt is combined with a cation group of the cationic copolyester in advance, so that the speed of the dye entering the cationic copolyester is reduced, and the aim of uniform dyeing is fulfilled.
Further, the pH regulator is at least one of acetic acid, citric acid, oxalic acid, hydrochloric acid and tartaric acid. In order to improve the level dyeing effect and increase the precision of the detection result, the compound pH regulator is preferably compounded by tartaric acid and acetic acid according to the mass volume ratio of 1-2 g:1 mL.
The invention relates to a method for rapidly detecting the content of a cationic copolyester modified monomer, which specifically comprises the following steps:
Accurately weighing 0.5-5 g of cationic dye, putting the cationic dye into a beaker, adding a proper amount of distilled water for dissolving, transferring the cationic dye into a 1L volumetric flask, adding 2-5 g of a compound slow-dyeing agent, adding a pH regulator, fixing the volume to a scale position by using distilled water, and shaking up to obtain a dye solution with the cationic dye concentration of 0.5-5 g/L and the compound slow-dyeing agent concentration of 2-5 g/L, pH being 3.5-6.0.
Diluting the dye solution obtained in the step 1 until the concentration of the cationic dye is 10.00mg/L, and taking the dye solution as a standard solution mother solution; then quantitatively diluting the mother liquor to obtain a series of standard working solutions with different cationic dye concentrations;
scanning the mother solution of the standard solution by a spectrophotometer to determine the maximum absorption wavelength, and then measuring the absorbance values of a series of standard working solutions with different concentrations at the wavelength; and drawing a standard working curve by taking the cationic dye concentration of the standard working solution as an abscissa and the absorbance value as an ordinate.
In order to increase the precision of the detection result, screening the cationic copolyester to be detected by a mesh screen of 5-20 meshes to obtain cationic copolyester particles to be detected with uniform particle size; the screening particle size is basically consistent, so that the time required for the dye solution to permeate and diffuse into the particles is basically consistent when the particles are dyed in the dye solution, and the dyeing uniformity is ensured.
Placing 20-100 g of screened cationic copolyester particles to be detected in a conical flask, adding 500mL of the dye solution prepared in the step 1, heating the dye solution to 90-100 ℃ under the stirring condition (the stirring speed is controlled to be 50-200 rpm/min), carrying out heat preservation dyeing for 60-90 min, cooling to room temperature, and taking out the dyed cationic copolyester.
Taking and diluting the residual dyeing solution after dyeing, determining the absorbance value of the residual dyeing solution after dilution under the maximum absorption wavelength determined in the step 2, and determining the concentration of the cationic dye in the residual dyeing solution after dilution according to the standard working curve obtained in the step 2 so as to determine the concentration of the cationic dye in the residual dyeing solution before dilution;
determining the adsorption capacity of the modified monomer in the cationic copolyester to the cationic dye according to the concentration of the cationic dye in the residual dye solution, and obtaining the content of the modified monomer in the cationic copolyester according to the dyeing saturation value of the modified monomer to the cationic dye.
Further, in the step 1, the concentration range of the standard working solution is 0.00-10 mg/L.
Further, the absorbance in step 1 and step 4 is measured using distilled water as a reference solution.
Further, in the step 4, in order to ensure that the detection result precision and the absorbance have an additive principle, the residual dye solution after dyeing is diluted so that the absorbance is within the range of 0.2-0.8.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the accurate and rapid detection of the content of the cationic copolyester modified monomer is realized by the accurate quantitative dyeing method, the method has strong operability, high detection result precision and good repeatability, the accurate detection of cationic modified monomers with different contents can be met, the quantitative detection can be realized within 90min or less for the serial copolyesters with the cationic modified monomer content of 0.5-15%, and the relative standard deviation is less than or equal to 2%. Plays an important real-time detection feedback role in the product quality stability in the continuous production process.
Drawings
FIG. 1 is a graph showing the saturation values of dyeing solutions of several known cationic copolyesters with modified monomer content for different cationic red X-GRL concentrations.
FIG. 2 is a standard curve obtained in example 1 of the present invention.
Detailed Description
The following examples are given to illustrate the present invention, and the following examples are carried out on the premise of the technical solution of the present invention, and give detailed embodiments and specific procedures, but the scope of the present invention is not limited to the following examples.
The invention utilizes a spectrophotometry method to quickly detect the content of the modified monomer in the cationic copolyester. Spectrophotometry is a method of quantifying a substance to be measured by the absorbance of the substance at a specific wavelength or within a certain wavelength range. The instrument used in the examples described below was a dual beam UV-vis spectrophotometer UV 1902.
Example 1
In this example, the content of the modified monomer in the cationic copolyester is detected according to the following method:
Accurately weighing 1g of cationic dye (cationic red X-GRL), putting the cationic dye (cationic red X-GRL) into a small beaker, adding a small amount of water for dissolving, transferring the beaker into a 1L volumetric flask, adding 2g of a complex slow-dyeing agent consisting of sodium acetate and sodium chloride (the mass ratio is 2:1), adding a pH regulator consisting of tartaric acid and acetic acid (the mass-volume ratio is 2g:1mL), finally fixing the volume to a scale position by using distilled water, and shaking up to obtain a dye solution with the cationic dye concentration of 1g/L and the complex slow-dyeing agent concentration of 2g/L, pH-5.5.
And (3) diluting the dye liquor obtained in the step (1) until the concentration of the cationic dye is 10.00mg/L, and taking the dye liquor as a mother liquor of a standard solution.
Transferring 10mL of mother liquor into a 50mL volumetric flask, diluting to a scale, and shaking up. Pouring the diluted mother solution into a 3cm absorption cell, selecting 'wavelength scanning' in a spectrophotometer by taking deionized water as a reference solution, and performing wavelength scanning on the mother solution of the standard solution to determine the maximum absorption wavelength of the mother solution.
Sequentially adding 10.00mg/L of standard dye liquor mother liquor 0.00, 2.00, 4.00, 6.00, 8.00 and 10.00(mL) into 6 50mL volumetric flasks, diluting the solution to a marked line by using pure water, and shaking the solution uniformly to obtain standard working solutions with the concentrations of 0.00, 0.40, 0.80, 1.20, 1.60 and 2.00mg/L respectively; then, deionized water is used as a reference solution, and the absorbance value of each concentration standard working solution is measured at the maximum absorption wavelength; and (3) drawing a standard working curve by taking the cationic dye concentration of the standard working solution as an abscissa and the absorbance value as an ordinate, and fitting to obtain a dye solution standard curve equation as shown in figure 1: 0.2067C +0.0018, curve correlation coefficient R2The linear relationship is good at 0.9991. In the formula: a is the absorbance of the dye liquor, and C is the concentration of the cationic dye in the dye liquor. The absorbance A value of the dye liquor is better between 0.2 and 0.8, and the dye bath ratio is controlled to be well prepared.
Screening the cationic copolyester slices to be detected by using a 10-mesh stainless steel screen to obtain cationic copolyester particles (the weight of the hundred particles is 2.43 +/-0.30 g) with uniform particle size.
Placing 20g of screened cationic copolyester particles to be detected in a conical flask, adding 500mL of dye liquor with the cationic dye concentration of 1g/L prepared in the step 1, placing the dye liquor in a magnetic stirring rotor, placing the conical flask on an electromagnetic heating stirrer, starting heating and stirring, controlling the stirring speed to be 100rpm/min, heating the dye liquor to 100 ℃, preserving heat and dyeing for 70min, then cooling to room temperature, and taking out the dyed cationic copolyester to be detected.
And (3) taking 1mL of residual dye solution after dyeing into a 250mL volumetric flask, diluting to a scale, and shaking up. Determining the absorbance value of the residual dye liquor after dilution under the maximum absorption wavelength determined in the step 2 by using a 3cm absorption cell and deionized water as a reference solution, and determining the concentration of the cationic dye in the residual dye liquor after dilution according to the standard working curve obtained in the step 2, thereby determining the concentration of the cationic dye in the residual dye liquor before dilution;
determining the adsorption capacity of the modified monomer in the cationic copolyester to the cationic dye according to the concentration of the cationic dye in the residual dye solution, and obtaining the content of the modified monomer in the cationic copolyester according to the dyeing saturation value of the modified monomer to the cationic dye.
The cationic copolyester with 6 known modified monomer contents was tested as described above, and the results are shown in table 1.
TABLE 1
2 cationic copolyesters with known modified monomer contents of 10.00% and 12.00% were tested in 6 replicates, respectively, as described above, and the results are shown in Table 2.
TABLE 2
As can be seen from Table 2, the relative standard deviation of the results of 6 parallel tests on cationic copolyester chips with 2 different modified monomer contents is less than 2.0%. It can be seen that the method of the present invention is fast, accurate and precise.
Example 2
In this example, the content of the modified monomer in the cationic copolyester is detected according to the following method:
The same as in example 1.
The same as in example 1.
Accurately weighing cationic copolyester slices to be detected, and sieving the cationic copolyester slices with a 20-mesh stainless steel screen to obtain cationic copolyester particles (the weight of hundred particles is 2.43 +/-0.30 g) with uniform particle size.
Placing 30g of screened cationic copolyester particles to be detected in a conical flask, adding 400mL of dye liquor with the cationic dye concentration of 1g/L prepared in the step 1, placing the dye liquor in a magnetic stirring rotor, placing the conical flask on an electromagnetic heating stirrer, starting heating and stirring, controlling the stirring speed to be 50rpm/min, heating the dye liquor to 100 ℃, preserving heat and dyeing for 80min, cooling to room temperature, and taking out the dyed cationic copolyester to be detected.
And (3) taking 1mL of residual dye solution after dyeing into a 250mL volumetric flask, diluting to a scale, and shaking up. Determining the absorbance value of the residual dye liquor after dilution under the maximum absorption wavelength determined in the step 2 by using a 3cm absorption cell and deionized water as a reference solution, and determining the concentration of the cationic dye in the residual dye liquor after dilution according to the standard curve obtained in the step 2, thereby determining the concentration of the cationic dye in the residual dye liquor before dilution;
determining the adsorption capacity of the modified monomer in the cationic copolyester to the cationic dye according to the concentration of the cationic dye in the residual dye solution, and obtaining the content of the modified monomer in the cationic copolyester according to the dyeing saturation value of the modified monomer to the cationic dye.
The cationic copolyesters with 6 known modified monomer contents were tested as described above and the results are shown in table 3.
TABLE 3
2 cationic copolyesters with known modified monomer contents of 9.50% and 11.00% were tested in 6 replicates, respectively, as described above, and the results are shown in Table 4.
TABLE 4
As can be seen from Table 4, the relative standard deviation of the results of 6 parallel tests on cationic copolyester chips with 2 different modified monomer contents is less than 2.0%. It can be seen that the method of the present invention is fast, accurate and precise.
Example 3
In this example, the content of the modified monomer in the cationic copolyester is detected according to the following method:
Accurately weighing 1g of cationic dye (cationic red X-GRL), putting the cationic dye (cationic red X-GRL) into a small beaker, adding a small amount of water for dissolving, transferring the beaker into a 1L volumetric flask, adding 2g of a complex slow-dyeing agent consisting of sodium acetate and anhydrous sodium sulfate (the mass ratio is 2:1), adding a pH regulator consisting of tartaric acid and acetic acid (the mass-volume ratio is 2g:1mL), finally fixing the volume to a scale position by using distilled water, and shaking up to obtain a dye solution with the cationic dye concentration of 1g/L and the complex slow-dyeing agent concentration of 2g/L, pH-5.5.
The same as in example 2.
The same as in example 2.
The same as in example 2.
The same as in example 2.
The cationic copolyesters with 6 known modified monomer contents were tested as described above and the results are shown in table 5.
TABLE 5
2 cationic copolyesters with known modified monomer contents of 9.50% and 11.00% were tested in 6 replicates, respectively, as described above, and the results are shown in Table 6.
TABLE 6
As can be seen from Table 6, the relative standard deviation of the results of 6 parallel tests on cationic copolyester chips with 2 different modified monomer contents is greater than 2.0%. This is because the complex retarding agent used in example 3 is composed of sodium acetate and anhydrous sodium sulfate, which is different from the complex retarding agent composed of sodium acetate and sodium chloride in examples 1 and 2. Therefore, the compound slow-dyeing agent composed of sodium acetate and sodium chloride is preferred in the invention.
The above description is only exemplary of the present invention and should not be taken as limiting the invention, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. A rapid detection method for the content of a cationic copolyester modified monomer is characterized by comprising the following steps: adding to-be-detected cationic copolyester into dye liquor containing cationic dye with known concentration, adsorbing the cationic dye to saturation by using modified monomers in the cationic copolyester, measuring the absorbance of the residual dye liquor after adsorption by using a spectrophotometry, determining the concentration of the cationic dye in the residual dye liquor after adsorption, determining the adsorption amount of the modified monomers in the cationic copolyester to the cationic dye, and obtaining the content of the modified monomers in the cationic copolyester according to the dyeing saturation value of the modified monomers to the cationic dye.
2. The method for rapidly detecting the content of the cationic copolyester modified monomer according to claim 1, which is characterized in that: the dye solution containing the cationic dye is obtained by dissolving the cationic dye in deionized water, adding a complex retarding agent, and then adjusting the pH value to 3.5-6.0 by using a pH regulator; in the dye solution, the concentration of the cationic dye is 0.5-5 g/L, and the concentration of the compound slow-dyeing agent is 2-5 g/L.
3. The method for rapidly detecting the content of the cationic copolyester modified monomer according to claim 1 or 2, which is characterized by comprising the following steps: the compatibility value K of the cationic dye is 3-5.
4. The method for rapidly detecting the content of the cationic copolyester modified monomer according to claim 2, which is characterized in that: the compound slow-dyeing agent is prepared by compounding at least two of sodium acetate, sodium chloride, disodium hydrogen sulfate, disodium hydrogen phosphate, sodium dihydrogen phosphate and anhydrous sodium sulfate.
5. The method for rapidly detecting the content of the cationic copolyester modified monomer according to claim 4, which is characterized in that: the compound slow-dyeing agent is prepared by compounding sodium acetate and sodium chloride according to the mass ratio of 1-4: 0.5-2.
6. The method for rapidly detecting the content of the cationic copolyester modified monomer according to claim 2, which is characterized in that: the pH regulator is at least one of acetic acid, citric acid, oxalic acid, hydrochloric acid and tartaric acid.
7. The method for rapidly detecting the content of the cationic copolyester modified monomer according to claim 1, which is characterized by comprising the following steps:
step 1, dye liquor preparation
Accurately weighing 0.5-5 g of cationic dye, putting the cationic dye into a beaker, adding a proper amount of distilled water for dissolving, transferring the cationic dye into a 1L volumetric flask, adding 2-5 g of a compound slow-dyeing agent, adding a pH regulator, fixing the volume to a scale position by using distilled water, and shaking up to obtain a dye solution with the cationic dye concentration of 0.5-5 g/L and the compound slow-dyeing agent concentration of 2-5 g/L, pH being 3.5-6.0;
step 2, drawing a standard working curve
Diluting the dye solution obtained in the step 1 until the concentration of the cationic dye is 10.00mg/L, and taking the dye solution as a standard solution mother solution; then quantitatively diluting the mother liquor to obtain a series of standard working solutions with different cationic dye concentrations;
scanning the mother solution of the standard solution by a spectrophotometer to determine the maximum absorption wavelength, and then measuring the absorbance values of a series of standard working solutions with different concentrations at the wavelength; drawing a standard working curve by taking the cationic dye concentration of the standard working solution as an abscissa and the absorbance value as an ordinate;
step 3, treating the cationic copolyester to be detected
Screening the cationic copolyester to be detected by a mesh screen of 5-20 meshes to obtain cationic copolyester particles to be detected with uniform particle size;
step 4, dyeing of cationic copolyester to be detected
Placing 20-100 g of screened cationic copolyester particles to be detected in a conical flask, adding 500mL of the dye solution prepared in the step 1, heating the dye solution to 90-100 ℃ under the stirring condition, carrying out heat preservation dyeing for 60-90 min, cooling to room temperature, and taking out the dyed cationic copolyester to be detected;
step 5, detecting the content of the modified monomer in the cationic copolyester to be detected
Taking and diluting the residual dyeing solution after dyeing, determining the absorbance value of the residual dyeing solution after dilution under the maximum absorption wavelength determined in the step 2, and determining the concentration of the cationic dye in the residual dyeing solution after dilution according to the standard working curve obtained in the step 2 so as to determine the concentration of the cationic dye in the residual dyeing solution before dilution;
determining the adsorption capacity of the modified monomer in the cationic copolyester to the cationic dye according to the concentration of the cationic dye in the residual dye solution, and obtaining the content of the modified monomer in the cationic copolyester according to the dyeing saturation value of the modified monomer to the cationic dye.
8. The method for rapidly detecting the content of the cationic copolyester modified monomer according to claim 7, which is characterized in that: in the step 2, the concentration range of the standard working solution is 0.00-10 mg/L.
9. The method for rapidly detecting the content of the cationic copolyester modified monomer according to claim 7, which is characterized in that: in the step 5, diluting the residual dye liquor after dyeing until the absorbance of the dye liquor is in the range of 0.2-0.8.
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