Preparation method of fluorescent whitening agent

A fluorescent whitening agent and catalyst technology, applied in chemical instruments and methods, addition of luminescent/fluorescent substances, luminescent materials, etc., can solve problems such as poor compatibility of fluorescent whitening agents, achieve good whitening effect, convenient operation, The effect of good compatibility

Active Publication Date: 2014-01-22
SHANGHAI DONGSHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, with the rapid development of science and technology and the continuous improvement of papermaking technology, a number of high-tech value-added paper surface sizing agents have been born. At present, many new surface sizing agents have poor compatibility with fluorescent whitening agents. The existence of this technical problem has caused certain obstacles to how to apply high-tech value-added surface sizing agents

Method used

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  • Preparation method of fluorescent whitening agent
  • Preparation method of fluorescent whitening agent
  • Preparation method of fluorescent whitening agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] One, fluorescent whitening agent, its characteristic is prepared through the following steps;

[0018] (a). Chemical composition: 80 parts of 4-dimethylaminobenzoyl chloride, 100 parts of p-chloro-o-aminophenol, doped with SO 4 2－ ∕ZrO 2 -Fe 2 o 3 - SiO 2 3 parts of mixed crystal solid superacid catalyst, 150 parts of ethylene glycol monobutyl ether, 5 parts of sodium hydroxide;

[0019] (b) Preparation method: Add 4-dimethylaminobenzoyl chloride, p-chloro-o-aminophenol, doped SO 4 2－ ∕ZrO 2 -Fe 2 o 3 - SiO 2 Type mixed crystal solid superacid catalyst, ethylene glycol monobutyl ether, heat up to 160 ° C, reflux for 3 hours, stand still, separate the catalyst, add sodium hydroxide, then heat up to 100 ° C and continue stirring for 60 minutes, stand still, Separate and remove the lower layer solution, distill off the solvent from the upper layer reaction product by decompression method, make the reactant a jelly, add 100 parts of deionized water below 10°C, fi...

Embodiment 2

[0026] One, fluorescent whitening agent, its characteristic is prepared through the following steps;

[0027] (a). Chemical components: 90 parts of 4-dimethylaminobenzoyl chloride, 110 parts of p-chloro-o-aminophenol, doped

[0028] SO 4 2－ ∕ZrO 2 -Fe 2 o 3 - SiO 2 Type mixed crystal solid superacid catalyst 4 parts, ethylene glycol monobutyl ether 165 parts, sodium hydroxide 7.5 parts;

[0029] (b) Preparation method: Add 4-dimethylaminobenzoyl chloride, p-chloro-o-aminophenol, doped SO 4 2－ ∕ZrO 2 -Fe 2 o 3 - SiO 2 Type mixed crystal solid superacid catalyst, ethylene glycol monobutyl ether, heat up to 160-170°C, reflux for 2.5 hours, stand still, separate the catalyst, add sodium hydroxide, then heat up to 110°C and continue stirring for 60 minutes, stand still , Separation and removal of the lower layer solution, the upper layer reaction product is distilled off the solvent with a reduced pressure method, so that the reactant is a jelly, add 100 parts of deioni...

Embodiment 3

[0032] One, fluorescent whitening agent, its characteristic is prepared through the following steps;

[0033] (a). Chemical composition: 100 parts of 4-dimethylaminobenzoyl chloride, 120 parts of p-chloro-o-aminophenol, doped with SO 4 2－ ∕ZrO 2 -Fe 2 o 3 - SiO 2 Type mixed crystal solid superacid catalyst 5 parts, ethylene glycol monobutyl ether part 180 parts, sodium hydroxide 10 parts;

[0034] (b) Preparation method: Add 4-dimethylaminobenzoyl chloride, p-chloro-o-aminophenol, doped SO 42－ ∕ZrO 2 -Fe 2 o 3 - SiO 2 Type mixed crystal solid superacid catalyst, ethylene glycol monobutyl ether, heat up to 160-180°C, reflux for 3 hours, stand still, separate the catalyst, add sodium hydroxide, then heat up to 120°C and continue stirring for 60 minutes, stand still , Separation and removal of the lower layer solution, the upper layer reaction product is distilled off the solvent with a reduced pressure method, so that the reactant is a jelly, add 100 parts of deionized...

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Abstract

The invention provides a preparation method of a fluorescent whitening agent. The preparation method comprises the following steps: mixing 4-dimethylaminobenzoylchloride, p-chlorophenol ortho-aminophenol, doped SO42- / ZrO2-Fe2O3-SiO2 type mixed crystal solid superacid catalyst and ethylene glycol monobutyl ether, heating to 160-180 DEG C, performing reflux reaction for 2-3 hours, standing, separating the catalyst, adding 5-10 parts of sodium hydroxide, rising to 100-120 DEG C, stirring for 1-2 hours, standing, separating and removing the lower solution, distilling off a solvent from an upper reaction product through a decompression method, enabling the reactant to a jelly, adding water below 10 DEG C, washing and filtering, and obtaining the fluorescent whitening agent which is 2-(p-dimethylamino phenyl)-4-chlorine-benzoxazole. The preparation method of the fluorescent whitening agent is simple in process; the use of the strong acid is avoided, so that the corrosion to the equipment is avoided; the use of a large amount of water is avoided; the prepared fluorescent whitening agent is good in compatibility with a surface sizing agent in papermaking and good in whitening effect.

Description

technical field [0001] The invention relates to a preparation method of a fluorescent whitening agent. Background technique [0002] Fluorescent whitening agent can absorb invisible ultraviolet light (wavelength range is about 360-380nm), and convert it into blue light or purple visible light with longer wavelength, so it can compensate the unwanted yellowish light in the matrix, and at the same time reflect more than the original The incident wavelength is more visible light in the range of 400-600nm, so that the product appears whiter, brighter and more vivid. Fluorescent whitening agent is a kind of color conditioning agent, which has the function of brightening and brightening. It is widely used in many fields such as papermaking, textiles, and coatings. Fluorescent whitening agent with tetrasulfonic acid group, this kind of fluorescent whitening agent has excellent whitening effect and dispersibility in pulp. However, with the rapid development of science and technolo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D263/57D21H21/30C09B57/00C09K11/06
CPCC07D263/57C09B57/00C09K11/06C09K2211/1033D21H21/30
Inventor 施晓旦李改霞郭和森
Owner SHANGHAI DONGSHENG NEW MATERIALS
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