Light, heat, electronic beam acid generating source containing 2, 1, 4,- heavy nitrogen naphthaquinone sulfuryl and preparing process thereof
A technology of naphthoquinone sulfonyl chloride and electron beam, which is applied in the direction of photomechanical equipment, photoplate making process of pattern surface, and photosensitive material used in optomechanical equipment, etc.
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[0021] In the preparation method of the acid-generating source of the present invention, when utilizing the first type of material to synthesize 2,1,4-diazonaphthoquinone sulfonate compounds, a composite solvent must be used, such as dimethylformamide (DMF) and Acetone or a mixed solvent with dioxane in a weight ratio of 1:1. The solvent consumption is 5-10 times of reactant weight. The N-hydroxyimide compound and 2,1,4-diazonaphthoquinonesulfonyl chloride can be dissolved in a mixed solvent at one time, and then a tertiary amine catalyst is added dropwise at a temperature of 30-40°C; also The N-hydroxyimide compound can be dissolved in DMF first, the sulfonyl chloride compound can be dissolved in acetone or dioxane, and after mixing and stirring evenly, a tertiary amine catalyst is added dropwise for reaction. The tertiary amine catalyst used is preferably triethylamine or triethylenediamine, and its amount is greater than or equal to the mole number of 2,1,4-diazonaphthoqui...
Embodiment 1
[0030] Example 1 Synthesis of N-Hydroxyphthalimide (M-1)
[0031] Take 20 g (0.29 mol) of hydroxylamine hydrochloride, stir and dissolve in 78 ml of distilled water. Then slowly add 15.25 g (0.144 mol) of anhydrous sodium carbonate powder into the system. After it is completely dissolved, add 36.2g (0.24mol) of finely ground phthalic anhydride to the system in batches at 30-40°C. After the addition, raise the temperature of the system to above 90°C and maintain it for 30 minutes. Then cooling rapidly, a large amount of light yellow solid can be precipitated, suction filtered, washed, and dried at 60°C to obtain a light yellow needle-like solid with the structure shown in M-1, with a yield of 94%.
Embodiment 2
[0032] Example 2 Synthesis of N-Hydroxysuccinimide (M-2)
[0033] Take 10 g (0.14 mol) of hydroxylamine hydrochloride, stir and dissolve in 35 ml of water. Then slowly add 7.6g (0.07mol) of anhydrous sodium carbonate powder into the system. After all the solution was dissolved, 12.25 g (0.12 mol) of succinic anhydride was added in batches to the system at room temperature. After the addition, the temperature of the system was raised to reflux temperature, maintained for 2 hours, and then distilled to dryness under reduced pressure. Add 200ml of acetone to the flask, maintain the system at 40°C for extraction, and filter. The filtrate was concentrated, filtered, and dried at 60°C to obtain a yellow flaky or flesh-colored powder solid with the structure shown in M-2, and the yield was 67.4%.
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