CN112414954A - Method for testing iron ion chelating capacity suitable for actual production conditions of printing and dyeing mill - Google Patents
Method for testing iron ion chelating capacity suitable for actual production conditions of printing and dyeing mill Download PDFInfo
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- CN112414954A CN112414954A CN202011406124.1A CN202011406124A CN112414954A CN 112414954 A CN112414954 A CN 112414954A CN 202011406124 A CN202011406124 A CN 202011406124A CN 112414954 A CN112414954 A CN 112414954A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 57
- 238000012360 testing method Methods 0.000 title claims abstract description 29
- 238000004043 dyeing Methods 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 20
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 60
- 239000007864 aqueous solution Substances 0.000 claims abstract description 59
- 239000002270 dispersing agent Substances 0.000 claims abstract description 58
- -1 iron ion Chemical class 0.000 claims abstract description 48
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 45
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229960000583 acetic acid Drugs 0.000 claims abstract description 15
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 15
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 15
- 230000008859 change Effects 0.000 claims abstract description 10
- 230000007613 environmental effect Effects 0.000 claims abstract description 5
- 239000013522 chelant Substances 0.000 claims description 9
- 239000012085 test solution Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 4
- 230000009920 chelation Effects 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 9
- 238000010998 test method Methods 0.000 abstract description 8
- 239000002738 chelating agent Substances 0.000 description 5
- 230000002378 acidificating effect Effects 0.000 description 4
- 230000006872 improvement Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- G01N21/29—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using visual detection
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- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Coloring (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for testing iron ion chelating capacity suitable for actual production conditions of a printing and dyeing mill, which comprises the following steps: 1) preparing ferric trichloride aqueous solution with certain concentration; 2) taking three parts of prepared ferric trichloride aqueous solution with the same amount, and respectively adding the chelating dispersant with the same amount; 3) adding glacial acetic acid into one part of the ferric trichloride aqueous solution sample, using one part as blank comparison, and adding caustic soda into the other part; 4) standing the ferric trichloride aqueous solution obtained in the step 3) at normal temperature, respectively observing the appearance color change of the three aqueous solutions, and recording the standing time; 5) comparing the chelating speed of the chelating dispersant to iron ions under different environmental conditions; 6) and comparing the chelating capacity of the chelating dispersant, calculating the chelating capacity of the chelating dispersant on the iron ions, and expressing the chelating capacity of the sample on the iron ions. The test method is suitable for testing the iron chelating capacity of the chelating dispersant in a dye printing factory under different environmental conditions, is simple to operate, has intuitive effect, and is easy to popularize and use in the factory.
Description
Technical Field
The invention relates to a method for testing iron ion chelating capacity suitable for actual production conditions of a printing and dyeing mill, belonging to the technical field of textiles.
Background
The chelating dispersant is a high-efficiency multipurpose organic chelate which can soften water and can be used for Ca2+、Mg2+、Fe3+The metal ions have chelating force and scum dispersing force, prevent the generation of precipitate and scum produced by other dirt in the dyeing and finishing process, and can slowly dissolve and remove the silicon scale in the equipmentCalcium soap precipitate and oligomer can prevent the re-contamination of metal salt to various fiber, raise the whiteness, brightness and color fastness of bleached, dyed and printed product and prevent the re-contamination of white bottom of printed and color-dyed product. Chelating dispersants play a very important role in the textile printing industry.
At present, the determination of chelated Fe3+The method for testing the capacity is different, the testing is generally carried out under the condition of acidity or pH value of 11-12, and the testing results have larger difference. The three methods as described in "test method for measuring ability to chelate iron ion" at the 7 th stage of volume 26 of printing and dyeing auxiliary "test each have advantages and disadvantages under specific acidic conditions; fe (OH) described in brief introduction to method for measuring chelate iron chelate value of chelating agent and evaluation of "dyeing auxiliary agent" at volume 27, 103In the process of titration by using a precipitation method, 20 percent NaOH solution is needed to maintain the pH of the test solution to be 12; the iron content detection kit from Merck adds an acidic buffer to the assay. Therefore, the common test method for the iron ion chelating capacity has relatively large limitation, and if the chelating dispersant is used under different pH conditions (acidic, neutral and alkaline), the chelating capacity of the chelating dispersant to iron has certain difference, so the test data of the test method can only be used as reference.
The invention is mainly directed to chelating Fe3+The capacity measurement is more suitable for the actual production environment of a printing and dyeing mill, and can be used for testing under different pH values (different production procedures and different pH conditions in the actual production of the printing and dyeing mill). The test method provided by the invention is used for testing the iron chelating capacity, is more suitable for the actual production environment of a printing and dyeing mill, can visually observe the iron chelating effect under different acidic, neutral and alkaline conditions, and avoids the influence of the test environment on the iron chelating capacity test.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the method for testing the iron ion chelating capacity, which is suitable for the actual production conditions of the printing and dyeing mill, and has the advantages of simple operation, intuitive phenomenon and easy popularization and application in the mill.
In order to achieve the purpose, the invention adopts a method for testing the iron ion chelating capacity suitable for the actual production conditions of a printing and dyeing mill, which comprises the following steps:
1) taking analytically pure FeCl3﹒6H2Preparing an O sample into a ferric trichloride aqueous solution with a certain concentration;
2) taking three parts of prepared ferric trichloride aqueous solution with the same amount, respectively adding the chelating dispersant with the same amount, and uniformly stirring;
3) adding glacial acetic acid into one part of the three parts of ferric trichloride aqueous solution samples obtained in the step 2), taking the other part as blank comparison, and adding caustic soda into the other part to simulate the production conditions of a printing and dyeing mill;
4) standing the ferric trichloride aqueous solution obtained in the step 3) at normal temperature, respectively observing the appearance color change of the three aqueous solutions, and recording the standing time for the ferric trichloride aqueous solution to change from light yellow to colorless;
5) comparing the chelation speed of the chelating dispersant on iron ions under different environmental conditions according to the time for changing the ferric trichloride aqueous solution from light yellow to colorless;
6) comparing the chelating capacity of the chelating dispersant with the dosage of the ferric trichloride solution changed from light yellow to colorless chelating dispersant, then calculating the chelating capacity of the chelating dispersant to iron ions according to the formula (1), and expressing the amount of the chelating dispersant to the iron ions by a sample:
in the formula: w (Fe) -ability to chelate iron ions, mg/g;
m 1-FeCl contained in test solution3﹒6H2Mass of O, g;
m 2-mass of chelating dispersant in the test solution, g.
As an improvement, the concentration of the ferric trichloride aqueous solution prepared in the step 1) is 0.1-0.5 g/L.
In the step 2), three parts of the prepared ferric trichloride aqueous solution are taken, wherein each part is 200ml, and the dosage of the chelating dispersant is 1-4 g/L.
As an improvement, in the step 3), glacial acetic acid is added to be in an industrial grade, the content is more than 98%, and the using amount is 0.1-2.0 g/L; the added caustic soda is industrial grade, the content is more than 96 percent, and the dosage is 0-50 g/L.
As a modification, in the step 4), the time points of changing the light yellow of the ferric trichloride aqueous solution into colorless are recorded as 0min, 10min, 20min, 30min, 1h, 2h, 3h and 6 h.
The principle of the invention is as follows: the chelation effect on iron ions is a process of forming two or more coordination bonds between a chelating dispersant heavy-chelating ligand (containing two or more ligands with lone pair electrons) and iron ions to generate a coordination compound with a ring structure, and the strong binding effect of chelating agent molecules and the iron ions is utilized to chelate the iron ions into the chelating agent and change the iron ions into a stable compound with larger molecular weight, so that the solution is changed from light yellow to colorless.
Compared with the prior art, the invention has the beneficial effects that:
(1) the test method is suitable for testing the iron chelating capacity of the chelating dispersant in a dye printing factory under different environmental conditions, is simple to operate, has intuitive effect, and is easy to popularize and use in the factory.
(2) The test method only adopts the ferric chloride reagent, the glacial acetic acid and the caustic soda, does not need to additionally apply other chemical reagents for auxiliary test, and does not need to calibrate a standard solution.
(3) The testing method can qualitatively compare the advantages and disadvantages of the chelating dispersant on the iron ion chelating capacity, and is not only suitable for qualitatively comparing the iron ion chelating capacities of different chelating dispersants in the actual production of a printing and dyeing mill; the chelating ability of the chelating dispersant to iron ions can be quantitatively calculated according to the dosage of the test auxiliary.
Drawings
FIG. 1 is a graph showing the effect of chelating iron ions for 30min in example 1 of the present invention; wherein, (1) the sample is 0.25g/L ferric trichloride aqueous solution; (2) adding 2g/L of chelating dispersant into 0.25g/L ferric trichloride aqueous solution of a sample, and adjusting the pH value to be approximately equal to 4 by using glacial acetic acid; (3) adding 2g/L chelating dispersant into 0.25g/L ferric trichloride aqueous solution of a sample, and adjusting the pH value to be approximately equal to 7 by using glacial acetic acid/caustic soda; (4) adding 2g/L chelating dispersant into 0.25g/L ferric trichloride aqueous solution of a sample, and adjusting the pH value to be approximately equal to 14 by using caustic soda;
FIG. 2 is a graph showing the effect of chelating iron ions for 60min in example 1 of the present invention; wherein, (1) the sample is 0.25g/L ferric trichloride aqueous solution; (2) adding 2g/L of chelating dispersant into 0.25g/L ferric trichloride aqueous solution of a sample, and adjusting the pH value to be approximately equal to 4 by using glacial acetic acid; (3) adding 2g/L chelating dispersant into 0.25g/L ferric trichloride aqueous solution of a sample, and adjusting the pH value to be approximately equal to 7 by using glacial acetic acid/caustic soda; (4) adding 2g/L chelating dispersant into 0.25g/L ferric trichloride aqueous solution of a sample, and adjusting the pH value to be approximately equal to 14 by using caustic soda;
FIG. 3 is a graph showing the effect of chelating iron ions for 6 hours in example 1 of the present invention; wherein, (1) the sample is 0.25g/L ferric trichloride aqueous solution; (2) adding 2g/L of chelating dispersant into 0.25g/L ferric trichloride aqueous solution of a sample, and adjusting the pH value to be approximately equal to 4 by using glacial acetic acid; (3) adding 2g/L chelating dispersant into 0.25g/L ferric trichloride aqueous solution of a sample, and adjusting the pH value to be approximately equal to 7 by using glacial acetic acid/caustic soda; (4) the sample is 0.25g/L ferric trichloride aqueous solution, 2g/L chelating dispersant is added, and the pH value is adjusted to be approximately equal to 14 by caustic soda.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below. It should be understood, however, that the description herein of specific embodiments is only intended to illustrate the invention and not to limit the scope of the invention.
Example 1
A method for testing iron ion chelating ability suitable for actual production conditions of a printing and dyeing mill comprises the following steps:
1) taking analytically pure FeCl3﹒6H2Preparing an O sample into a ferric trichloride aqueous solution with the concentration of 0.25 g/L;
2) taking three 200ml portions of prepared ferric trichloride aqueous solution, respectively adding 2g/L chelating dispersant (such as chelating agent 580 (main component HEDP) produced by Zhanzhanfeng chemical industry, Guangdong province), and stirring well;
3) adding glacial acetic acid (industrial grade, content is more than 98%) 0.5g/L (pH is approximately equal to 4) into one part of the three parts of ferric trichloride aqueous solution samples obtained in the step 2), adjusting the pH value (pH is approximately equal to 7) of the other part of the three parts of ferric trichloride aqueous solution samples, and adding caustic soda (industrial grade, content is more than 96%) 10g/L (pH is 13-14) into the other part of the three parts of ferric trichloride aqueous solution samples;
4) standing the ferric trichloride aqueous solution obtained in the step 3) at normal temperature, respectively observing the appearance color change of three aqueous solutions, and recording the color changes of the solutions for 0min, 10min, 20min, 30min, 1h, 2h, 3h and 6 h;
5) when glacial acetic acid is 0.5g/L (pH is approximately equal to 4), the time for changing the ferric trichloride aqueous solution from light yellow to colorless is 30 min; when the pH value is not adjusted (pH is approximately equal to 7), the time for changing the ferric trichloride aqueous solution from light yellow to colorless is 6 h; when the pH value of caustic soda is 10g/L (13-14), the time for changing the light yellow of the ferric trichloride aqueous solution into colorless is 1 h;
6) comparing the chelating capacity of the chelating dispersant with the dosage of the ferric trichloride solution changed from light yellow to colorless chelating dispersant, then calculating the chelating capacity of the chelating dispersant to iron ions according to the formula (1), and expressing the amount of the chelating dispersant to the iron ions by a sample:
in the formula: w (Fe) -ability to chelate iron ions, mg/g;
m 1-FeCl contained in test solution3﹒6H2Mass of O, g;
m 2-mass of chelating dispersant in the test solution, g.
Example 1 is a parallel test of samples with the same amount of chelating dispersant under different pH values, and the chelating rates of the chelating dispersant on iron ions under different pH values can be compared. The specific iron ion chelating effect is shown in fig. 1-3, and analysis shows that the test method is practical.
Example 2
A method for testing iron ion chelating ability suitable for actual production conditions of a printing and dyeing mill comprises the following steps:
1) taking analytically pure FeCl3﹒6H2Preparing an O sample into a ferric trichloride aqueous solution with the concentration of 0.25 g/L;
2) taking four 200ml portions of prepared ferric trichloride aqueous solution, respectively adding 1.5g/L, 1.8g/L, 2g/L and 2.2g/L of chelating dispersant (such as chelating agent 580, produced by Zhanyuanfeng chemical industry in Guangdong), and stirring uniformly;
3) adding glacial acetic acid (industrial grade, content is more than 98%) 0.5g/L (pH is approximately equal to 4) into four parts of ferric trichloride aqueous solution samples obtained in the step 2);
4) standing the ferric trichloride aqueous solution obtained in the step 3) at normal temperature, observing and recording the time of the color change of the ferric trichloride aqueous solution, and respectively recording the color change of the ferric trichloride aqueous solution for 0min, 10min, 20min, 30min, 1h, 2h, 3h and 6 h;
5) the dosage of the chelating dispersant is 1.5g/L, and the ferric trichloride aqueous solution still presents light yellow after being placed for 6 hours;
the dosage of the chelating dispersant is 1.8g/L, the ferric trichloride aqueous solution still presents yellowish after being placed for 30min, and basically has no change after being placed for 6h, and iron ions can not be completely chelated;
the dosage of the chelating dispersant is 2g/L, and the time for changing the ferric trichloride aqueous solution from light yellow to colorless is 30 min;
the dosage of the chelating dispersant is 2.2g/L, and the time for changing the ferric trichloride aqueous solution from light yellow to colorless is about 25 min;
6) considering that the iron ions are completely chelated when the ferric trichloride aqueous solution is changed from light yellow to colorless, calculating the chelating capacity of the chelating dispersant on the iron ions according to the formula (1) according to the concentration of the ferric trichloride solution and the using amount of the chelating dispersant, and expressing the chelating capacity of the chelating dispersant on the iron ions by the amount of the sample chelating iron ions:
in the formula: w (Fe) -ability to chelate iron ions, mg/g;
m 1-FeCl contained in test solution3﹒6H2Mass of O, g;
m 2-mass of chelating dispersant in the test solution, g.
Example 2 is to adjust the dosage of the chelating dispersant under the same pH value (pH is approximately equal to 4), test and compare and calculate the chelating capacity of the chelating dispersant to iron ions.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (5)
1. A method for testing iron ion chelating ability suitable for actual production conditions of a printing and dyeing mill is characterized by comprising the following steps:
1) taking analytically pure FeCl3﹒6H2Preparing an O sample into a ferric trichloride aqueous solution with a certain concentration;
2) taking three parts of prepared ferric trichloride aqueous solution with the same amount, respectively adding the chelating dispersant with the same amount, and uniformly stirring;
3) adding glacial acetic acid into one part of the three parts of ferric trichloride aqueous solution samples obtained in the step 2), taking the other part as blank comparison, and adding caustic soda into the other part to simulate the production conditions of a printing and dyeing mill;
4) standing the ferric trichloride aqueous solution obtained in the step 3) at normal temperature, respectively observing the appearance color change of the three aqueous solutions, and recording the standing time for the ferric trichloride aqueous solution to change from light yellow to colorless;
5) comparing the chelation speed of the chelating dispersant on iron ions under different environmental conditions according to the time for changing the ferric trichloride aqueous solution from light yellow to colorless;
6) comparing the chelating capacity of the chelating dispersant with the dosage of the ferric trichloride solution changed from light yellow to colorless chelating dispersant, then calculating the chelating capacity of the chelating dispersant to iron ions according to the formula (1), and expressing the amount of the chelating dispersant to the iron ions by a sample:
in the formula: w (Fe) -ability to chelate iron ions, mg/g;
m 1-FeCl contained in test solution3﹒6H2Mass of O, g;
m 2-mass of chelating dispersant in the test solution, g.
2. The method for testing the iron ion chelating ability suitable for the actual production conditions of the printing and dyeing mill according to claim 1, wherein the concentration of the ferric trichloride aqueous solution prepared in the step 1) is 0.1-0.5 g/L.
3. The method for testing the iron ion chelating ability suitable for the actual production conditions of the printing and dyeing mill according to claim 1, wherein in the step 2), three parts of the prepared ferric trichloride aqueous solution are taken, each 200ml of the ferric trichloride aqueous solution is used, and the dosage of the chelating dispersant is 1-4 g/L.
4. The method for testing the iron ion chelating ability suitable for the actual production conditions of the printing and dyeing mill according to claim 1, wherein glacial acetic acid is added in the step 3) to be of industrial grade, the content is more than 98%, and the dosage is 0.1-2.0 g/L; the added caustic soda is industrial grade, the content is more than 96 percent, and the dosage is 0-50 g/L.
5. The method for testing the iron ion chelating ability suitable for the actual production conditions of the printing and dyeing mill as claimed in claim 1, wherein in the step 4), the time points of changing the light yellow of the ferric trichloride aqueous solution into colorless are recorded as 0min, 10min, 20min, 30min, 1h, 2h, 3h and 6 h.
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| CN113341063A (en) * | 2021-05-25 | 2021-09-03 | 贵州省产品质量检验检测院 | Method for measuring chelating capacity of agricultural ammonium polyphosphate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113341063A (en) * | 2021-05-25 | 2021-09-03 | 贵州省产品质量检验检测院 | Method for measuring chelating capacity of agricultural ammonium polyphosphate |
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