Aqueous phase synthesis method of tetraphenylphosphine phenate

A technology of tetraphenylphosphine phenoxide and tetraphenylphosphine halide, which is applied in the field of aqueous phase synthesis of tetraphenylphosphine phenoxide, can solve the problems of mother liquor recovery and treatment, unstable product components, and inability to continue production. Achieve strong operability and repeatability, easy control of reaction conditions, and avoid massive use and waste

Pending Publication Date: 2021-08-27
SHANDONG NORMAL UNIV EXPERIMENTAL PLANT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

First, tetraphenylphosphine bromide is synthesized, and then tetraphenylphosphine phenate is synthesized. The solvents used in the two steps are isopropanol and isobutanol respectively. The process operation is still relatively complicated and cannot be continuously produced.
And the second step reaction uses isobutanol as a solvent, washes and separates liquids with deionized water, and the separated water phase contains isobutanol, phenol, tetraphenylphosphine and NaBr, which needs further treatment; the washing operation takes away isobutanol Butanol also took away part of phenol, resulting in unstable product components and reduced product yield
[0004] Patent CN110272451A uses tetraphenylphosphine bromide and phenol as raw materials, methanol and water as solvents, and saves the operation of isobutanol liquid separation, but methanol has a high solubility to the product, and the single batch yield is 86%. The yield of the mother liquor has improved after the application of the mother liquor, but the mother liquor still contains a large amount of products and NaBr, and there is a problem of mother liquor recovery and treatment in the later stage

Method used

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  • Aqueous phase synthesis method of tetraphenylphosphine phenate
  • Aqueous phase synthesis method of tetraphenylphosphine phenate
  • Aqueous phase synthesis method of tetraphenylphosphine phenate

Examples

Experimental program
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Effect test

Embodiment 1

[0027] A kind of aqueous phase synthetic method of tetraphenylphosphine phenate, concrete steps are as follows:

[0028] In the autoclave, drop into triphenylphosphine (524.5g, 2.0mol), bromobenzene (376.8g, 2.4mol) and catalyst NiBr 2 (4.4g, 0.02mol), the temperature was raised to 160°C, the reaction pressure was 0.3MPa, and a developer was added (the developer was petroleum ether and ethyl acetate with a volume ratio of 2:1), used to soak the TLC plate, and TLC monitoring No remaining triphenylphosphine is the end of the reaction, and tetraphenylphosphine bromide is generated. After the reaction, the temperature was lowered to 100°C, and the excess bromobenzene was recovered by distillation under reduced pressure. During the distillation, appropriate pure water was added to take out the bromobenzene. After bromobenzene is completely distilled, put pure water into the reaction kettle and stir to completely dissolve tetraphenylphosphine bromide, then add sodium hydroxide to a...

Embodiment 2

[0030] In the autoclave, drop into triphenylphosphine (524.5g, 2.0mol), chlorobenzene (337.7g, 3.0mol) and catalyst NiCl 2 (2.6g, 0.02mol), the temperature was raised to 150°C, the reaction pressure was 0.4MPa, and the developer was added (the developer was petroleum ether and ethyl acetate with a volume ratio of 2:1), used to soak the TLC plate, and TLC monitoring No remaining triphenylphosphine is the end of the reaction, and tetraphenylphosphine chloride is generated. After the reaction, the temperature was lowered to 100°C, and the excess chlorobenzene was recovered by distillation under reduced pressure. During the distillation, pure water was added to take out the chlorobenzene, and the recovered chlorobenzene was subjected to liquid separation treatment and applied to the next batch of reactions. After the chlorobenzene is completely distilled, put pure water into the reaction kettle and stir to dissolve the tetraphenylphosphine chloride completely, then add potassium h...

Embodiment 3

[0032] In the autoclave, drop into triphenylphosphine (524.6g, 2.0mol), chlorobenzene (562.8g, 5.0mol) and catalyst PdCl 2 (8.9g, 0.05mol), the temperature was raised to 200°C, the reaction pressure was 1.0MPa, and the developer was added (the developer was petroleum ether and ethyl acetate with a volume ratio of 2:1), used to soak the TLC plate, and TLC monitoring No remaining triphenylphosphine is the end of the reaction, and tetraphenylphosphine fluoride is generated. After the reaction, the temperature was lowered to 110°C, and the excess fluorobenzene was recovered by atmospheric distillation. During the distillation, pure water was added to take out the fluorobenzene, and the recovered fluorobenzene was subjected to liquid separation treatment and applied to the next batch of reactions. After the fluorobenzene is completely distilled, put pure water into the reaction kettle and stir to dissolve the tetraphenylphosphine fluoride completely, then add potassium carbonate to...

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Abstract

The invention discloses an aqueous phase synthesis method of tetraphenylphosphine phenate. The preparation method comprises the following steps: subjecting triphenylphosphine to reacting with excessive halogenated benzene at certain temperature and pressure in the presence of a catalyst; after the reaction is finished, recovering the excessive halogenated benzene through distillation; then adding a certain amount of water to dissolve generated tetraphenylphosphine halide, and adjusting the pH value of an aqueous tetraphenylphosphine halide solution to be greater than 7 so as to allow the catalyst to be separated out in a precipitate form; and mixing the purified tetraphenylphosphine halide solution with phenol and caustic soda liquid, conducting reacting at a certain temperature, and carrying out heating dissolution, cooling crystallization, centrifugation and drying on the material liquid after the reaction is completed to finally obtain a tetraphenylphosphine phenate product. According to the invention, the above reactions are carried out in a pure water phase, and the tetraphenylphosphine phenolate product with high purity and stable components can be obtained; and meanwhile, the method has the advantages of environment-friendly process, simplicity in operation and high economic benefit.

Description

technical field [0001] The present invention relates to the preparation method of tetraphenylphosphine phenate, in particular to a kind of aqueous phase synthesis method of tetraphenylphosphine phenate. Background technique [0002] Tetraphenylphosphine phenate is a catalyst for thermoplastic polycarbonate synthesis, and it is an important industrial raw material. The production method of tetraphenylphosphine phenoxide is disclosed by DE-A19727351 and WO001 / 46100, mainly adopting tetraphenylphosphine bromide and phenol as raw materials and reacting with alcohols as solvent. Subsequent studies focused on optimizing the process for the reaction solvent and raw material ratio, but none of them substantially solved the problems of high raw material cost, complicated operation and inability to produce continuously. [0003] Patent CN109942628A discloses a synthesis method of tetraphenylphosphine phenate, which uses triphenylphosphine, bromobenzene and phenol as production raw ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/54
CPCC07F9/5442
Inventor 刘启奎毛震刘群杨松
Owner SHANDONG NORMAL UNIV EXPERIMENTAL PLANT CO LTD
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