Polyurethane-based black polymeric dye, preparing method and application

A polymer dye and polyurethane-based technology, which is applied in the field of polyurethane-based black polymer dye preparation, can solve the problems of complicated reaction process and difficult separation and purification, and achieve high color fixation rate, convenient use and easy film formation

Active Publication Date: 2016-09-21
ANHUI UNIVERSITY OF ARCHITECTURE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reaction process is relatively complicated, separation and pur

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0027] Example 1

[0028] In N 2 Under protection, add 100 g, 0.1 mol polytetrahydrofuran glycol to a four-necked flask equipped with a stirrer, condenser, and thermometer, and perform dehydration treatment for 2 hours at 110°C and 0.1 MPa.

[0029] The temperature was lowered to 70°C, 44.5g, 0.2mol isophorone diisocyanate, 40ml N-methylpyrrolidone and 0.02g dibutyltin dilaurate were added dropwise, and the reaction was carried out at 90°C for 3 hours.

[0030] Then 11.3g, 0.043mol disperse diazo black GNN was added, and the temperature was raised to 60℃ to react for 2h.

[0031] Then add 0.53g, 0.005mol diethylene glycol, and react at 60°C for 1 hour.

[0032] Finally, the N-methylpyrrolidone is removed by vacuum distillation to obtain a polyurethane-based black polymer dye.

[0033] The strongest ultraviolet absorption peak of the obtained product is 510nm, the thermal decomposition temperature in the first stage is 250-360°C, the thermal decomposition temperature in the second stage i...

Example Embodiment

[0034] Example 2

[0035] In N 2 Under protection, add 100 g, 0.1 mol of polycaprolactone diol to a four-necked flask equipped with a stirrer, a condenser, and a thermometer, and perform dehydration treatment for 2 hours at 110°C and 0.1 MPa.

[0036] Cool to 70°C, 50g, 0.2mol 4,4-diphenylmethane diisocyanate (MDI), 20ml dioxane and 0.02g stannous octoate, react at 90°C for 3 hours.

[0037] Then add 18.5g, 0.022mol Direct Fast Black G, and react at 50℃ for 2h.

[0038] Then add 0.45g, 0.005mol of 1,4-butanediol (), and react at 50°C for 1 hour.

[0039] Finally, the N-methylpyrrolidone is removed by vacuum distillation to obtain a polyurethane-based black polymer dye.

[0040] The strongest ultraviolet absorption peak of the obtained product is 520nm, the thermal decomposition temperature in the first stage is 265-380°C, the thermal decomposition temperature in the second stage is 380-550°C, and the glass transition temperature is 66°C.

Example Embodiment

[0041] Example 3

[0042] Into a flask equipped with a thermometer, a stirrer, a reflux condenser and a dropping funnel, add 100 g, 0.1 mol of polyoxypropylene glycol, and conduct dehydration treatment for 1.5 hours at 110° C. and 0.1 MPa.

[0043] The temperature was lowered to 80°C, 34.8g, 0.2mol toluene diisocyanate, 20ml butanone and 0.02g stannous octoate were added dropwise, and the reaction was carried out at 90°C for 3 hours.

[0044] Subsequently, 11g, 0.043mol disperse diazo black 3BF was added, and the temperature was raised to 60°C to react for 2h.

[0045] Then add 0.32g, 0.005mol ethylene glycol, and react at 60°C for 1 hour.

[0046] Finally, the N-methylpyrrolidone is removed by vacuum distillation to obtain a polyurethane-based black polymer dye.

[0047] The strongest ultraviolet absorption peak of the obtained product is 530nm, the thermal decomposition temperature in the first stage is 255-350°C, the thermal decomposition temperature in the second stage is 350-550°C, ...

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PUM

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Abstract

The invention discloses polyurethane-based black polymeric dye, a preparing method and application. The preparing method includes the steps that polymer polyol is heated to 90-110 DEG C and dehydrated for 1-2 h with the vacuum degree smaller than or equal to 0.1 MPa, and nitrogen is introduced for protection; the product is cooled to 60-80 DEG C, and isocyanate and a catalyst are added to react for 1-3 h at the temperature of 60-90 DEG C; micromolecular black dye, solvent and a catalyst are added and react for 3-8 h at the temperature of 60-90 DEG C to prepare a polyurethane prepolymer with black dye; chain extender is added and reacts for 1-3 h at the temperature of 50-90 DEG C; finally, the solvent is removed in vacuum. According to the prepared polyurethane-based black polymeric dye, the micromolecular black dye is directly added into the polyurethane chain, the content of the micromolecular black dye in the polyurethane can be adjusted according to needs, and therefore dye amount is controllable to meet requirements of different dyeing processes. The polyurethane-based black polymeric dye can be mixed with other kinds of dye for color matching and is suitable for various kinds of color and luster dying with a wide color spectrum.

Description

technical field [0001] The invention relates to a polymer dye, in particular to a polyurethane-based black polymer dye, a preparation method and an application. Background technique [0002] Small molecule black dyes play a very important role in the fields of printing and dyeing, leather, painting, medicine and so on. Due to the weak binding force of small molecule dyes, low dye utilization rate, lack of migration resistance, heat resistance and solvent resistance, and serious environmental pollution during use, the application in various fields is limited. . [0003] The early small molecular black dyes were mainly derived from azo benzidine, which had the advantages of good blackness, high dyeing rate and color fixation rate, but carcinogenic benzidine intermediates would be produced during production and use. In the 1970s, all black dyes derived from benzidine were banned. Although the dye is still used in developing countries, production of benzidine dyes has ceased ...

Claims

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Application Information

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IPC IPC(8): C08G18/66C08G18/48C08G18/42C08G18/10C08G18/32C09B69/10
CPCC08G18/10C08G18/4277C08G18/4825C08G18/4854C09B69/106C08G18/3206
Inventor 胡先海丁运生程从亮刘瑾陈建利
Owner ANHUI UNIVERSITY OF ARCHITECTURE
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