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Preparation method of stilbene ester polymerized fluorescent brightening and brightening agent

A stilbene, fluorescent brightening technology, applied in the direction of zinc halide, zirconia, etc., can solve the problems of old color performance, affecting color brightening and beauty, etc., to achieve convenient operation, excellent protection, and corrosion-free Effect

Active Publication Date: 2016-04-06
SHANGHAI DONGSHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the limitation of application technology, the function of fluorescent whitening agent as other color brightening and brightening conditioning agents has not been fully explored. The whitening agent that can really match other pigments has yet to be developed. The main problem is that although some Fluorescent whitening agents do have the effect of brightening and brightening other three colors, but the actual effect is that the color performance has an old feeling, which affects the beauty of brightening and brightening colors

Method used

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  • Preparation method of stilbene ester polymerized fluorescent brightening and brightening agent
  • Preparation method of stilbene ester polymerized fluorescent brightening and brightening agent
  • Preparation method of stilbene ester polymerized fluorescent brightening and brightening agent

Examples

Experimental program
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Effect test

Embodiment 1

[0022] 1. Synthesis steps of stilbene ester polymerized fluorescent brightening and brightening agent:

[0023] (a) Chemical composition: 120 parts of 4,4'-stilbene dicarboxylic acid, 50 parts of anhydrous methanol, 100 parts of phenylmalonic acid, 40 parts of 1,4-butanediol, 50 parts of polyethylene glycol, 0.2 parts of 98% concentrated sulfuric acid, doped with SO 4 2－ / ZrO 2 - 6 parts of AgCl type mixed crystal solid acid catalyst, 0.03 parts of molybdenum trichloride, 10 parts of sodium hydroxide;

[0024] (b) Preparation method: Add 120 parts of 4,4'-stilbene dicarboxylic acid, 50 parts of anhydrous methanol, doped SO 4 2－ / ZrO 2 - 6 parts of AgCl type mixed crystal solid acid catalyst, 0.2 part of 98% concentrated sulfuric acid, heat up to 80°C, reflux for 6 hours, the reflux tube needs to be cooled with 7°C ice water, stand still after reaction, and separate the lower layer solution;

[0025] (c) Take the upper liquid of the reaction in (b), add 100 parts of pheny...

Embodiment 2

[0034] 1. Synthesis steps of stilbene ester polymerized fluorescent brightening and brightening agent:

[0035] (a) Chemical composition: 150 parts of 4,4'-stilbene dicarboxylic acid, 30 parts of anhydrous methanol, 150 parts of phenylmalonic acid, 20 parts of 1,4-butanediol, 100 parts of polyethylene glycol, 0.1 part of 98% concentrated sulfuric acid, doped with SO 4 2－ / ZrO 2 - 10 parts of AgCl type mixed crystal solid acid catalyst, 0.01 part of molybdenum trichloride, 20 parts of sodium hydroxide;

[0036] (b) Preparation method: Add 150 parts of 4,4'-stilbene dicarboxylic acid, 30 parts of anhydrous methanol, doped SO 4 2－ / ZrO 2 -10 parts of AgCl type mixed crystal solid acid catalyst, 0.1 part of 98% concentrated sulfuric acid, heat up to 90°C, reflux for 4 hours, the reflux tube needs to be cooled with ice water at 5°C, stand still after reaction, and separate the lower layer solution;

[0037] (c) Take the upper liquid of the reaction in (b), add 150 parts of ph...

Embodiment 3

[0041] 1. Synthesis steps of stilbene ester polymerized fluorescent brightening brightening agent:

[0042] (a) Chemical composition: 135 parts of 4,4'-stilbene dicarboxylic acid, 40 parts of anhydrous methanol, 125 parts of phenylmalonic acid, 30 parts of 1,4-butanediol, 75 parts of polyethylene glycol, 0.15 parts of 98% concentrated sulfuric acid, doped with SO 4 2－ / ZrO 2 -AgCl type mixed crystal solid acid catalyst 8 parts, molybdenum trichloride 0.02 part, sodium hydroxide 15 parts;

[0043](b) Preparation method: Add 135 parts of 4,4'-stilbene dicarboxylic acid, 40 parts of anhydrous methanol, doped SO 4 2－ / ZrO 2 -8 parts of AgCl type mixed crystal solid acid catalyst, 0.15 parts of 98% concentrated sulfuric acid, heat up to 85°C, reflux for 5 hours, the reflux tube needs to be cooled with ice water at 6°C, stand still after reaction, and separate the lower layer solution;

[0044] (c) Take the upper liquid of the reaction in (b), add 125 parts of phenylmalonic ac...

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Abstract

The invention discloses a method for preparing a toluylene ester polymeric type fluorescence brightening and coloring agent. The method comprises the following steps: mixing 4,4-toluylene dioctyl phthalate, absolute methanol, a doped SO42- / ZrO2-AgC1 type mixed crystal solid acid catalyst and concentrated sulfuric acid, carrying out heating reflux reaction, standing after the reaction, adding phenylmalonic acid, 1,4-butanediol, polyethylene glycol and molybdenum trichloride, carrying out heating reflux reaction again, and post-treating the liquid at the upper layer after the reaction so as to obtain the toluylene ester polymeric type fluorescence brightening and coloring agent. The method is simple in process and convenient to operate, and corrosion of strong acids to equipment and application of a great deal of water resource is avoided. The fluorescence brightening and coloring agent prepared by using the method is used together with pigments of other colors, is applied to coatings, paper-making and stone paper production, has remarkable brightening and coloring functions on blue, green and red lights, and also has an excellent protection function on organic pigments.

Description

technical field [0001] The invention relates to a preparation method of a stilbene ester polymerized fluorescent brightening and brightening agent. Background technique [0002] Fluorescent whitening agent can absorb invisible ultraviolet light (wavelength range is about 360-380nm), convert it into blue light or purple visible light with longer wavelength, and reflect more than the original incident wavelength in the range of 400-600nm visible light, so that the product appears whiter, brighter, and more vivid. Fluorescent whitening agent is also a color conditioning agent. It has the effect of brightening and brightening in combination with other three-color pigments. In many fields, such as making green more bright and red more beautiful. However, due to the limitation of application technology, the function of fluorescent whitening agent as other color brightening and brightening conditioning agents has not been fully explored, and the whitening agent that can really mat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/676C08G63/85C08G63/83C01G25/02C01G9/04
Inventor 施晓旦郭和森
Owner SHANGHAI DONGSHENG NEW MATERIALS
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