A kind of polyurethane-based black polymer dye, preparation 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 high blackness

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 high blackness

CN105949425BActive Publication Date: 2019-01-15ANHUI UNIVERSITY OF ARCHITECTURE
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] in N 2 Under protection, add 100 g, 0.1 mol polytetrahydrofuran diol into a four-neck flask equipped with a stirrer, a condenser, and a thermometer, and dehydrate for 2 hours at 110° C. and 0.1 MPa.

[0029] Cool down to 70°C, add dropwise 44.5g, 0.2mol of isophorone diisocyanate, 40ml of N-methylpyrrolidone and 0.02g of dibutyltin dilaurate, and react at 90°C for 3 hours.

[0030] Then add 11.3g, 0.043mol disperse diazonium black GNN, raise the temperature to 60°C and react for 2h.

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

[0032] Finally, the N-methylpyrrolidone is distilled off under reduced pressure to obtain the polyurethane-based black polymer dye.

[0033] The strongest ultraviolet absorption peak of the obtained product is 510nm, the thermal decomposition temperature of the first stage is 250-360°C, the thermal decomposition temperature of the second stage is 360-550°C, and the glass transition temperature is 59...

Embodiment 2

[0035] in N 2 Under protection, add 100 g, 0.1 mol polycaprolactone diol into a four-necked flask equipped with a stirrer, a condenser, and a thermometer, and dehydrate for 2 hours at 110° C. and 0.1 MPa.

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

[0037] Then 18.5 g, 0.022 mol of direct suntan G was added, and the temperature was lowered to 50° C. for 2 hours.

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

[0039] Finally, the N-methylpyrrolidone is distilled off under reduced pressure to obtain the polyurethane-based black polymer dye.

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

Embodiment 3

[0042] To 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 dehydrate for 1.5 h at 110° C. and 0.1 MPa.

[0043] Cool down to 80°C, add dropwise 34.8g, 0.2mol toluene diisocyanate, 20ml methyl ethyl ketone and 0.02g stannous octoate, and react at 90°C for 3 hours.

[0044] Then add 11 g, 0.043 mol of dispersed diazonium black 3BF, and raise the temperature to 60° C. for 2 h.

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

[0046] Finally, the N-methylpyrrolidone is distilled off under reduced pressure to obtain the polyurethane-based black polymer dye.

[0047] The strongest ultraviolet absorption peak of the obtained product is 530nm, the thermal decomposition temperature of the first stage is 255-350°C, the thermal decomposition temperature of the second stage is 350-550°C, and the glass transition temperature is 61°C.

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Abstract

The invention discloses a polyurethane-based black polymer dye, a preparation method and an application thereof. The temperature of the polymer polyol is raised to 90-110°C, the vacuum degree is ≤0.1MPa, the dehydration treatment is carried out for 1-2 hours, and nitrogen protection is introduced; the temperature is lowered. To 60-80°C, add isocyanate and catalyst to react at 60-90°C for 1-3 hours; then add small molecule black dye, solvent and catalyst, react at 60-90°C for 3-8 hours to prepare polyurethane with black dye Prepolymer; then add a chain extender, react at 50-90°C for 1-3 hours; finally remove the solvent in vacuum. The polyurethane-based black polymer dye prepared by the invention is to insert the small molecule black dye into the polyurethane chain, and the content of the small molecule black dye in the polyurethane chain can be adjusted as required, so as to realize the controllable amount of the dye. Adapt to different dyeing process requirements. It can be blended and matched with other dyes, and it is suitable for dyeing a variety of colors with a wide 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

Patent Timeline
15 Jan 2019
Publication
CN105949425B
IPC
C08G18/66; C08G18/48; C08G18/42; C08G18/10; C08G18/32; C09B69/10
CPC
C08G18/10; C08G18/4277; C08G18/4825; C08G18/4854; C09B69/106; C08G18/3206
Inventors
胡先海; 丁运生