Method for preparing color masterbatch with natural dye

Patent metadata

Field	Value
Publication number	US-11535718-B2
Application number	US-202017294702-A
Country	US
Kind code	B2
Filing date	Oct 14, 2020
Priority date	Aug 11, 2020
Publication date	Dec 27, 2022
Grant date	Dec 27, 2022

Abstract

A method for preparing a color masterbatch with a natural dye is disclosed. The new method uses a phase change material tetradecane as one of the solvents to extract the natural dye, the extracted natural dye as a core material, and polybutylene succinate as a wall material to microencapsulate the natural dye containing the phase change material by a solvent evaporation method to prepare natural dye microcapsules, then melt-blends with a carrier resin, extrudes and granulates to obtain the color masterbatch with the natural dye. The microencapsulation improves the thermal stability of natural dye and compatibility with carrier resin The obtained color masterbatch with natural dye has excellent heat resistance, and the fabric obtained after spinning with it has good color fastness to hot pressing.

First claim

What is claimed is:

1. A method for preparing a color masterbatch with a natural dye, comprising: taking a mixed solvent of a phase change material tetradecane and ethanol to extract the natural dye, taking polybutylene succinate as a wall material to microencapsulate the natural dye containing the phase change material by a solvent evaporation method to obtain natural dye/tetradecane microcapsules, then melt-blending the natural dye/tetradecane microcapsules with a carrier resin to obtain a mixed product. extruding and granulating the mixed product to obtain the color masterbatch with the natural dye.

2. The method for preparing the color masterbatch with the natural dye according to claim 1 , wherein the method comprises the following specific steps:
(1) removing impurities of a natural plant raw material, cleaning, drying the natural plant raw material in the air to obtain a cleaned natural plant raw material. crushing the cleaned natural plant raw material into 80-200 mesh to obtain a natural plant powder, and soaking the natural plant powder in the mixed solvent of the phase change material tetradecane and the ethanol for 1-2 h to obtain a first mixture, extracting under a reflux and filtering the first mixture, extracting the first mixture 3-5 times repeatedly to obtain extracted solutions, combining the extracted solutions obtained from multiple times of extraction to obtain a. natural dye stock solution; removing the ethanol by decompression distillation to obtain a tetradecane-containing natural dye solution;
(2) dissolving the polybutylene succinate into 100 mL chloroform, adding the tetradecane-containing natural dye solution obtained in step (1) to obtain a second mixture, stirring the second mixture at a predetermined speed, and mixing the second mixture uniformly to obtain a chloroform solution of the polybutylene succinate containing the natural dye;
(3) adding 100 mL deionized water, Arabic gum and sodium dodecylbenzene sulfonate into a 250 mL three-port flask to obtain a third mixture, fully stirring and dissolving the third mixture;
adding the chloroform solution of the polybutylene succinate containing the natural dye obtained in step (2) into the three-port flask to obtain a fourth mixture. slowly raising a temperature of the fourth mixture to 40-50° C., condensing and recovering steam of the fourth mixture, keeping at the temperature of 40-50° C. for 4-6 h, forming microcapsules by a gradual solidification of the polybutylene succinate caused by an evaporation of the chloroform, collecting solids, fully cleaning with deionized water and drying the solids to obtain natural dye/tetradecane microcapsules; and
(4) adding 10-25 parts by weight of the natural dye/tetradecane microcapsules, 0.5-1.5 parts by weight of an antioxidant and 70-90 parts by weight of a carrier resin to a high-speed mixer for a mixing to obtain a well-mixed material, and adding the well-mixed material into a twin-screw extruder for a melt blending, an extrusion and agranulation to obtain a resulting product; after cooling the resulting product with 25-30° C. water, pelletizing and drying the resulting product at 80-100° C. to obtain the color masterbatch with the natural dye.

3. The method for preparing the color masterbatch with the natural dye according to claim 2 , wherein the natural plant raw material in step (1) is one selected from the group consisting of rhubarb, turmeric, red pepper, camphor leaves, madder, and vervain, and a volume ratio of the tetradecane to the ethanol is 1:5-2:5.

4. The method for preparing the color masterbatch with the natural dye according to claim 2 , wherein in step (1), a temperature of the reflux is 60-100° C., and a time of the reflux is 0.5-2 h.

5. The method for preparing the color masterbatch with the natural dye according to claim 2 , wherein in step (2), a mass ratio of the tetradecane-containing natural dye solution to the polybutylene succinate is 3:1-5:1.

6. The method for preparing the color masterbatch with the natural dye according to claim 2 , wherein in step (3), a mass ratio of the Arabic gum and the sodium dodecylbenzene sulfonate is 1:3-1:6, and a total mass of the Arabic gum and the sodium dodecylbenzene sulfonate accounts for 2%-4% of a total mass of the third mixture.

7. The method for preparing the color masterbatch with the natural dye according to claim 2 , wherein in step (4), the antioxidant is antioxidant 1010, and the carrier resin is ethylene terephthalate.

8. The method for preparing the color masterbatch with the natural dye according to claim 2 , wherein in step (4), a rotation speed of the high-speed mixer is 500-1,500 rpm, a temperature of the mixing is 150-180° C., and a time of the mixing is 10-30 min.

9. The method for preparing the color masterbatch with the natural dye according to claim 2 , wherein in step (4), screw temperatures of the extrusion and the granulation are set as follows: 200-250° C. in a first zone, 230-255° C. in a second zone, 220-260° C. in a third zone, 220-260° C. in a fourth zone, 220-260° C. in a fifth zone and 220-260° C. in a sixth zone.

Assignees

• Univ Changzhou

Inventors

• Chen Qun
• Peng Yonggang
• Ji Junling
• Chen Haiqun
• Wang Yuan
• Tan Junjie

Classifications

• C08K5/1345

  Carboxylic esters of phenolcarboxylic acids · CPC title

• C08J3/226 Primary

  using a polymer as a carrier · CPC title

• D01F1/06 Primary

  Dyes · CPC title

• C08K5/0041

  Optical brightening agents, organic pigments · CPC title

• C08J3/126

  Polymer particles coated by polymer, e.g. core shell structures · CPC title