- Novel synthesis method of clean and safe photoinitiator (2,4,6-trimethylbenzoyldiphenyl-diphenylphosphine oxide)
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The invention relates to the technical field of synthesis of photoinitiators, in particular to a novel synthesis method of a clean and safe photoinitiator (2,4,6-trimethylbenzoyldiphenyl-diphenylphosphine oxide). The method includes the steps of evenly mixing anhydrous alcohol with N-methylimidazole at the room temperature, raising the temperature to 30-50%, controlling the temperature, dropwise adding diphenylphosphine oxide, raising the temperature to 50-100 DEG C, conducting the constant-temperature reaction for 2-3 h, conducting standing and layering to take supernatant liquid for decompressing and distilling to obtain diphenyl alkoxylphosphine, making the diphenyl alkoxylphosphine start to react with 2,4,6-trimethylbenzoyldiphenyl chloride at the controlled temperature of 50 DEG C under the vacuum condition of -0.098 Mpa, raising the temperature by 10 DEG C every 20 minutes until the temperature is raised to 90 DEG C, conducting the constant-temperature reaction for 4-8 h, and adding 50% ethyl alcohol crystals to obtain a target product. The produced byproduct is subjected to vacuum removal and then enters a tail gas recovery system to be recovered through two stages of condensation. The synthesis method is simple in step, safe, clean, low in running cost and high in byproduct recovery rate.
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Paragraph 0049; 0050
(2019/06/12)
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- Alkyl arylphosphinites
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A process for the preparation of alkyl arylphosphinites of the formula (I) STR1 in which R1 is (C1 -C16)-alkyl, cyclohexyl, cyclopentyl, aryl which can also be substituted by halogen, (C1 -C6)-alkoxy groups R2 is aryl which can also be substituted by halogen, (C1 -C6)-alkyl, (C1 -C6)-alkoxy groups, where R1 and R2 together with the phosphorous atom can also form a ring and R3 is (C1 -C4)-alkyl, which comprises reacting halo(aryl) phosphines of the formula (II) STR2 in which R1, R2 have the meaning given above and X is halogen, with ammonia-containing alcohols of the formula (III) in which R3 has the meaning given above.
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