Preparation method of diazo photosensitizer

A technology of photosensitizer and diazo, which is applied in the direction of photomechanical equipment, photoplate making process of patterned surface, optics, etc., can solve the problems of long period of photosensitizer, poor quality of photosensitizer, and the need for cooling in the preparation process, so as to reduce the Drying steps, short production cycle, reduced synthesis and drying process effects

Pending Publication Date: 2021-01-29
浙江荣生科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to address the above-mentioned deficiencies in the prior art technology, and provide a kind of simple and stable synthesis and preparation method of diazo photosensitizer, which effectively solves the long cycle of preparing photosensitizer, and the preparation process needs to be cooled down, The obtained photosensitizer has poor quality and other problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 320g of concentrated sulfuric acid and 160g of phosphoric acid successively in a 1000ml three-necked flask, cool down in a water bath at room temperature, and gradually add 150g of wet p-aminodiphenylamine diazosulfate (VRT, with a purity of 60-65%), and control the temperature below 40°C. Subsequently, 9 g of paraformaldehyde was added, and the temperature was controlled below 40° C. for 3 h. The reaction solution was slowly added to 1800g of water to dissolve, and 15g of zinc chloride and 92g of sodium chloride were added to precipitate a yellow precipitate, which was filtered and dried to obtain 100g of a photosensitizer product.

Embodiment 2

[0022] Add 275g of concentrated sulfuric acid and 205g of phosphoric acid in sequence to a 1000ml three-neck flask, cool down in a water bath at room temperature, gradually add 150g of wet p-aminodiphenylamine diazosulfate, control the temperature below 40°C, then add 9g of paraformaldehyde, and control the temperature at React below 40°C for 3h. The reaction solution was slowly added to 1600g of water for dissolution, and 15g of zinc chloride and 92g of sodium chloride were added to precipitate a yellow precipitate, which was filtered and dried to obtain 95g of photosensitizer product.

Embodiment 3

[0024] Add 320g of concentrated sulfuric acid and 160g of phosphoric acid in sequence to a 1000ml three-neck flask, cool down in a water bath at room temperature, gradually add 150g of wet p-aminodiphenylamine diazonium chloride salt, control the temperature below 40°C, then add 11g of paraformaldehyde, and control the temperature at React below 40°C for 3h. The reaction solution was slowly added to 1800g of water for dissolution, and 15g of zinc chloride and 92g of sodium chloride were added to precipitate a yellow precipitate, which was filtered and dried to obtain 102g of photosensitizer product.

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PUM

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Abstract

The invention discloses a preparation method of a diazonium photosensitizer, which comprises the following steps: 1) mixing concentrated sulfuric acid and phosphoric acid according to a proper ratio to obtain a mixed acid, cooling, and slowly adding a proper amount of p-aminodiphenylamine diazonium sulfate (VRT) which is a wet product; wherein the temperature is controlled to be 20-40 DEG C when the p-aminodiphenylamine diazonium sulfate is added; 2) slowly adding a proper amount of paraformaldehyde after the dissolution in the step 1) is finished, and reacting at the temperature of below 40 DEG C until the reaction is complete; 3) dissolving a reaction solution completely reacted in the step 2) in water, adding a proper amount of a chlorine salt, and separating out a yellow precipitate; and 4) filtering, and drying the yellow precipitate to obtain the product. According to the preparation method disclosed by the invention, reaction with paraformaldehyde is carried out in the mixed acid, the reaction temperature can be effectively increased, the direct damage effect of the concentrated sulfuric acid on the raw materials is reduced, the reaction can be carried out at a relatively high temperature which is easier to control, the weight of the synthesized photosensitizer required for photoresist mixing is reduced to 90%, and the cost is saved.

Description

Technical field: [0001] The invention relates to the technical field of polymer material synthesis, in particular to a simple and stable preparation method of a diazo photosensitizer. Background technique: [0002] As people's awareness of environmental protection continues to increase, it has become an inevitable trend for product replacement to replace heavy chrome photosensitive glue with diazo photosensitive glue. In the current market, most of the photosensitizers of flat screen photosensitive adhesives that are commonly used are diazo photosensitizers, and the synthesis of the photosensitizers is mostly using VRT aqueous solution to first synthesize diazo double salts. The dried diazonium double salts are mixed with paraformaldehyde in concentrated sulfuric acid at 15 ℃ below the reaction, washed with ethanol to obtain the available diazo photosensitizer. The process is cumbersome, the cycle of preparing the photosensitizer is long, and the preparation process needs t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G12/08G03F7/021
CPCC08G12/08G03F7/021
Inventor 刘日生刘今
Owner 浙江荣生科技有限公司
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