- High performance liquid phase continuous automatic production and co-production technology of organic phosphine compound
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The invention relates to the field of photocuring functional new material chemicals, and discloses a high performance liquid phase streamline type continuous automatic production technology of an acylphosphine oxide organic phosphine compound for the first time, which not only can produce a single specific target product, but also can co-produce a product mixture of two or more than two of the products of the type. The process technology has outstanding low-cost economic competitiveness and environment-friendly characteristics for large-scale manufacturing of target products. The target product comprises sym-trimethylbenzoyl diphenyl phosphine oxide (also known as 2, 4, 6-trimethylbenzoyl diphenyl phosphine oxide, trade name TPO), sym-trimethylbenzoyl phenyl ethyl phosphonate (trade name TPO-L) and structural analogues thereof, and a mixture of the sym-trimethylbenzoyl diphenyl phosphine oxide and the sym-trimethylbenzoyl phenyl ethyl phosphonate. The organic phosphine compound is an olefinic bond-containing (C=C) unsaturated radiation polymerization system photoinitiator and/or flame retardant and the like with wide application.
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Paragraph 0077-0078
(2021/05/12)
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- Preparation method of methyl substituted benzaldehyde
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The invention relates to a preparation method of methyl substituted benzaldehyde, in particular to a method for preparing alkyl aromatic aldehyde through a carbonylation reaction by adopting methyl substituted aromatic hydrocarbon as raw materials. According to the method, ionic liquid with the high catalytic activity is adopted, and methyl substituted benzene is used for preparing the methyl substituted benzaldehyde under the alleviated condition with high conversion rate; meanwhile, the reaction time is shortened, waste water, gas and industrial residues are reduced, and no auxiliaries withhigh corrosivity are adopted.
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Paragraph 0067-0069
(2021/03/06)
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- Chlorosilane-Catalyzed Coupling of Hydrogen Phosphine Oxides with Acyl Chlorides Generating Acylphosphine Oxides
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We report a new method for the synthesis of acylphosphine oxides by the direct coupling of hydrogen phosphine oxides and acyl chlorides mediated by chlorosilanes. This new protocol is greener and safer, because it precludes the generation of volatile haloalkanes and the use of oxidants employed in the conventional methods. Moreover, moisture-unstable acylphosphine oxides that are difficult to prepare via the conventional methods can be generated using this new method.
- Zhang, Jian-Qiu,Han, Li-Biao
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supporting information
p. 4633 - 4637
(2020/06/23)
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- New preparation method of first-class phenyl phosphine oxide initiator
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The invention provides a new preparation method of a first-class phenyl phosphine oxide initiator. The method comprises the steps that (1) benzene and aluminum trichloride are added into a reaction vessel and stirred uniformly, then phosphorus trichloride is added, the temperature is slowly increased, and after a complete reaction, the temperature is reduced to room temperature; (2) a reaction mixture obtained in the step (1) is slowly added dropwise into a solvent containing a decomplexing agent, and the temperature is controlled for decomplexing; (3) a decomplexing product obtained in the step (2) is filtered to separate solids, and filtrate is subjected to pressure reduction distillation to obtain phenyl dialkoxy phosphine or diphenyl alkoxy phosphine; (4) a product obtained in the step(3) is dissolved in a benzene or methylbenzene solvent, and a trichloromethyl acetyl compound is added dropwise for a reaction; and (5) a solution obtained after the complete reaction in the step (4)is subjected to low-pressure desolvation, and light-yellow liquid or solid, namely the phenyl phosphine oxide initiator, is obtained through crystallization, suction filtering and drying. The methodhas the advantages that raw materials are easy to obtain, cost is low, operation is easy to perform, and mass production can be realized.
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- Preparation method for high-purity ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate
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The invention discloses a preparation method for high-purity ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate. The preparation method comprises the following concrete steps: reacting phenylphosphinate with aromatic aldehyde so as to prepare an intermediate, subjecting the intermediate to catalytic oxidation so as to obtain benzoylphenylphosphinic acid and subjecting benzoylphenylphosphinic acid and diethyl sulfate to an ethylation reaction so as to obtain ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate. According to the invention, raw materials have high quality and stable properties; by-produced impurities produced during synthesis of ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate can be removed through neutralization, and ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate with a purity of higher than 99.0%, which meets market demands for the high-purity photoinitiator ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate.
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Paragraph 0012; 0019; 0020; 0021; 0022; 0023; 0024-0026
(2017/10/13)
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- 2, 4, 6-trimethyl benzoyl phenyl phosphinic acid ethyl ester preparation method
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The invention relates to a preparation method of 2,4,6-trimethyl benzoyl phenyl ethyl phosphonate, and in particular relates to a method for preparing 2,4,6-trimethyl benzoyl phenyl ethyl phosphonate through the steps of carrying out substitution condensation reaction on dichlorophenyl phosphine and ethanol to obtain an intermediate; performing condensation reaction on the intermediate and 2,4,6-trimethyl benzaldehyde under an alkaline condition, and finally performing oxidation by using an oxidant under catalysis of a catalyst. The preparation process of 2,4,6-trimethyl benzoyl phenyl ethyl phosphonate, disclosed by the invention, has the advantages as follows: the influences of an acidic medium on the intermediate can be avoided; the requirements of the condensation reaction between 2,4,6-trimethyl benzaldehyde and phenyl ethyl hypophosphite for reaction equipment can be reduced; meanwhile, the reaction yield can be ensured; the preparation process is simple in operation and is suitable for industrial production.
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Paragraph 0027; 0028; 0029
(2017/03/14)
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- Preparation of α-carbonylphosphine oxides
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The preparation of α-carbonylphosphine oxides by oxidizing an α-hydroxyalkyl phosphine oxide with an organic hydroperoxide or of an organic peroxy acid in the presence of a compound of a Group IV to Group VIII metal in the periodic table, and novel α-hydroxybenzyl phosphine oxides. α-Carbonylphosphine oxides are used as photoinitiators for polymerizable compositions.
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