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Solvent-based yellow dye for environment-friendly fluorescent pigment

A fluorescent pigment and solvent-based technology, applied in the direction of coumarin dyes, etc., can solve the problems of high pollution, unsuitable for industrial production, difficult recovery of solvents, and low yield, and achieve high product yield, simplified operation, and high recovery rate Effect

Active Publication Date: 2013-07-10
WANLONG CHEM
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  • Claims
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AI Technical Summary

Problems solved by technology

[0006] Comparing the advantages and disadvantages of several processes, the first, second and third methods require more than three steps of reaction, the operation is complicated, and the yield is not high
Although the fourth method requires only one step of synthesis, it needs to add a large amount of lye to purify, the solvent is difficult to recover, and the pollution is too large to be suitable for industrial production.

Method used

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Examples

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Effect test

Embodiment 1

[0014] Solvent-type yellow dye for environmentally friendly fluorescent pigments, the raw material ratio is: ethyl cyanoacetate: ethanol: hydrogen chloride: 4-chloro-2-aminophenol: 4-N,N-diethylamino salicylaldehyde: catalyst = 1 :0.5-0.6:0.9-1.05:0.95-1.0:0.05-0.2. Its preparation method: add ethyl cyanoacetate absolute alcohol into the solvent, dissolve it into benzene, toluene or xylene, control the temperature between 5-25 degrees, pass in hydrogen chloride gas, 4-8 hours, and age for 8 to 24 hours, filter. Use C1 to C8 alcohol as solvent to react the filtered material with 4-chloro-2-aminophenol, 4-N,N-diethylaminosalicylaldehyde and catalyst at room temperature for 0.5 to 2 hours, then heat up to Reflux and heat preservation for 2 to 8 hours, filter and dry to obtain solvent-type yellow dye 1601.

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Abstract

The invention relates to a solvent-based yellow dye for an environment-friendly fluorescent pigment. The ratio of raw materials is as follows: ethyl cyanoacetate:ethanol:hydrogen chloride:4-chlorine-2-aminophenol:4-N,N-diethylaminosalicylaldehyde:catalyst=1:(0.5-0.6):(0.9-1.05):(0.95-1.0):(0.05-0.2). A solvent-based yellow dye preparation method comprises the following steps: adding the ethyl cyanoacetate and absolute alcohol to a solvent, wherein the solvent is benzene, toluene or xylene, and the temperature is controlled in the range from 5 DEG C and 25 DEG C; introducing the hydrogen chloride for 4-8 hours, keeping the constant temperature for 8-24 hours, and then filtering; and with a C1-C8 alcohol as a solvent, reacting the filtered material with 4-chlorine-2-aminophenol, the 4-N,N-diethylaminosalicylaldehyde and the catalyst for 0.5-2 hours at a room temperature, then raising the temperature to a backflow temperature, and filtering and drying after heat preservation for 2-8 hours to obtain the solvent-based yellow dye (160:1). Compared with the conventional process, the method is relatively simplified in operation, less in three wastes, high in product yield, high in quality, simple in solvent recovery and high in recovery ratio.

Description

technical field [0001] The invention relates to high-tech fields such as environment-friendly fluorescent pigments, plastic coloring, colored fluorescent resins for solar concentrators, photosensitive materials, photosensitive materials, and optical disc recording materials. Background technique [0002] The existing 1,4-N,N-diethylamino salicylaldehyde and diethyl malonate condensation ring closure method [0003] 2. 3-N,N-diethylaminophenol and diethyl ethoxymethylene malonate in catalyst TiCl 4 closed ring method [0004] 3. Benzoxazole ring, 4-N,N-diethylamino salicylaldehyde condensation method [0005] 4. One-pot synthesis of ethyl cyanoacetate, 4-N,N-diethylamino salicylaldehyde and o-aminophenol [0006] Comparing the advantages and disadvantages of several processes, the first, second and third methods require more than three steps of reaction, the operation is complicated, and the yield is not high. Although the fourth method only needs one step of synthesi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B57/02
Inventor 陈权弟
Owner WANLONG CHEM
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