Preparation method of black waterborne polyurethane dye

A technology for water-based polyurethane and black dye, applied in the field of water-based polyurethane, can solve the problems of low phenolic hydroxyl activity, uncontrollable, limited amount of chromophore access, and achieve high color fastness, good durability, and improved washing resistance. Effect

Active Publication Date: 2015-01-07
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

China's "Functional Materials" (2011, Volume 42, No. 2, Page 351-354) reported that on the basis of using the active dihydroxyl group contained in the acid medium black T (EBT) structure, it can be used as a chain extender. The chromophore was introduced into the polyurethane molecular chain to prepare a TDI black water-based polyurethane dye (EBT-PU). However, due to the low activity of the phenolic hydroxyl group, the amount of the chromophore incorporated was limited and uncontrollable.

Method used

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  • Preparation method of black waterborne polyurethane dye
  • Preparation method of black waterborne polyurethane dye
  • Preparation method of black waterborne polyurethane dye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 2.65 grams of chloroethanol, 0.25 grams of sodium hydroxide, 0.05 grams of sodium iodide and 1.21 grams of chrome black T into 70 milliliters of water, and keep it at 90 °C for 12 hours after completely dissolving, and slowly add 1.5 milliliters of mass percent to the reaction system Concentrated hydrochloric acid with a concentration of 37%; after the reaction, remove 70% of the added water at 60°C and 0.01MPa vacuum, and the filtered precipitate is washed with 10ml of water and dried in a vacuum oven to constant weight to obtain black Solid chrome black T-type pink light black diol EBT-BDiol;

[0035] 14 grams of number average molecular weight M n PTMG of 2000 was dehydrated at 110°C for 1 hour, cooled to 50°C, added 7 grams of IPDI, stirred and reacted at 80°C for 2 hours, then added 0.48 grams of EBT-BDiol prepared above, 1.5 grams of DMPA, 0.9 grams of BDO, 0.01 grams of DBTDL and 10 grams of methyl ethyl ketone, the constant temperature was cooled to 20 DEG ...

Embodiment 2

[0046] Add 2.84 grams of chloroethanol, 0.2 grams of sodium hydroxide, 0.05 grams of sodium iodide and 1.25 grams of amino black 10B into 70 ml of water, and keep it at 90°C for 24 hours after being completely dissolved; slowly add 2 ml of mass percent to the reaction system Concentrated hydrochloric acid with a concentration of 37%; after the reaction, 80% of the added water was pumped out under 60°C and 0.01MPa vacuum conditions; the filtered precipitate was washed with 10ml of water and dried in a vacuum oven to constant weight to obtain black Solid amino black 10B type blue violet light black diol AB10B-BDiol;

[0047] 14 grams of number average molecular weight M n PPG of 2000 was dehydrated at 110°C for 1 hour and then cooled to 50°C, added 5.45 grams of TDI, stirred and reacted at 80°C for 2 hours, then added 0.48 grams of the above-prepared AB10B-BDiol, 1.5 grams of DMPA, 1.05 grams of DEG, and 0.01 grams of DBTDL and 10 grams of acetone, stirred and reacted at a cons...

Embodiment 3

[0054] Add 1.3 grams of chloroethanol, 0.25 grams of potassium carbonate, 0.04 grams of sodium iodide and 0.75 grams of Sudan Black B into 70 milliliters of acetone, raise the temperature to 60°C and keep it warm for 18 hours; after the reaction, add 200 milliliters of water to the reaction system until precipitation Precipitation, the filtered precipitate was washed with 20ml of water and then dried in a vacuum oven to constant weight to obtain a black solid Sudan Black B-type blue light black diol SBB-BDiol;

[0055] 14 grams of number average molecular weight M n The PCL of 2000 was dehydrated at 110°C for 1 hour, then cooled to 50°C, added 7 grams of IPDI, stirred and reacted at 80°C for 2 hours, and then added 0.42 grams of the above-prepared SBB-BDiol, 0.4 grams of BDO, 0.01 grams of DBTDL and 10 grams of Acetone, keep the temperature at 70°C for 5 hours and then cool down to 55°C; then add dropwise a mixed solution of 1.9 grams of MDEA and 5 grams of acetone within 2 ho...

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Abstract

The invention discloses a preparation method of a black waterborne polyurethane dye based on black chromophores in diols. The preparation method is characterized by comprising the following steps of enabling activated hydrogen in amino groups or hydroxyls contained in molecular structures of three black dyes to react with chloroethanol to obtain three black diols; then, combining the black diols with micromolecular diols, and partially or completely substituting the micromolecular diols; and next, reacting with diisocyanate, macromolecular diols and a hydrophilic chain extender to obtain the black waterborne polyurethane dye. By using the method, other micromolecular chain extenders can be partially or completely substituted with the black diols, so that solid content of an emulsion is wide in distribution range and adjustable, and the content of the black chromophores in a molecular chain of polyurethane can be controlled as required; and meanwhile, the black chromophores enter the molecular chain of the dye in a chemical bonding way, so that the characteristics of high temperature resistance, solvent resistance and migration resistance of a macromolecular dye can be sufficiently exerted, and the dye is good in durability, high in color fastness and good in safety.

Description

technical field [0001] The invention belongs to the technical field of water-based polyurethane, and in particular relates to the synthesis of diols with black chromophores and a preparation method for using the diols to partially or completely replace common diols to form black water-based polyurethane dyes. Background technique [0002] In textile, printing, printing and dyeing, leather and other fields, small molecular black dyes are widely used as one of the most used dyes. Since the general small molecular dyes are usually fixed on the dyed material through ionic bonds, hydrogen bonds, van der Waals force, etc., the binding force with the dyed material is not strong, and it is easy to migrate to the material during placement, washing, dry cleaning, use, etc. surface, causing constant peeling and fading. In addition, although the azo-based black dyes derived from benzidine have the advantages of good blackness, high dyeing rate and color fixation rate, they will release...

Claims

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Application Information

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IPC IPC(8): C08G18/66C08G18/32C08G18/48C08G18/42C09B43/28C09B67/22
CPCC08G18/0814C08G18/0823C08G18/3836C08G18/3857C08G18/4277C08G18/4854C08G18/664C08G18/6692C09B69/106
Inventor 张兴元孙伟许海燕
Owner UNIV OF SCI & TECH OF CHINA
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