High performance liquid phase continuous automatic production and co-production technology of organic phosphine compound

A high-efficiency liquid phase and compound technology, which is applied in organic chemistry, bulk chemical production, and compounds of Group 5/15 elements of the periodic table, etc., can solve problems such as high cost, unrealized continuous automatic production, and environmental protection and hazardous waste.

Pending Publication Date: 2021-05-11
SHENZHEN UV-CHEMTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above-mentioned known literature technologies have been proved to have significant process defects one by one, including but not limited to the following aspects: the use of phosphorus trichloride, benzene, aluminum trichloride and other hazardous raw materials, high cost of process routes, and many environmentally hazardous wastes, The use of highly air-sensitive and thus expensive and hazardous alkali metal or organometallic reagents; the use of highly air-sensitive and foul-smelling organophosphonane raw materials or intermediates; the use of highly polluting main group metal and/or transition metal oxidation catalysts, Accelerators, or decomplexers (patents CN201310099065 and CN2011104264185), etc.; use of inorganic or organic peroxides with explosion risks as terminal ox...

Method used

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  • High performance liquid phase continuous automatic production and co-production technology of organic phosphine compound
  • High performance liquid phase continuous automatic production and co-production technology of organic phosphine compound
  • High performance liquid phase continuous automatic production and co-production technology of organic phosphine compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070]Example 1: High performance liquid phase flow line continuous automation production TPO

[0071][Aryl halide phosphine section] Under nitrogen protection, 66 kilograms of yellow phosphorus is placed in a pressure-resistant reactor, and 375 kg of chlorobenzene and 190 kg phenyl dichloride, mixture itself is sequentially added from the automatic metering infusion tank. When the pressure conditions were heated to 340-360 degrees Celsius for 4 hours, the reaction system was cooled to room temperature, and the liquid phase mixture was directly automatically input, and the hierarchical distillation device was opened, and the distillation was first distilled at normal pressure to obtain about 90 kg of chlorobenzene and three. The mixture of phosphorus chloride (used), and the restriction remissions were collected in sequentially collected from 235 kg of phenylphrachlorphrachloride (recovery) and 233 kg of diphenylphosphine. [Arylylphosphonate section] Under nitrogen protection, the 233 ...

Embodiment 2

[0072]Example 2: High performance liquid phase flow line continuous automation production TPO

[0073]The step of repeating the first example, but using an equal amount of 66 kg of grinding red phosphorus instead of the yellow phosphorus, heating is left in a aryl halide phosphine process to 390 degrees Celsius. After the streamlined process is completed, the TPO finished product is approximately 289 kg.

Embodiment 3

[0074]Example 3: High-performance liquid phase flow line continuous automation production TPO

[0075][Aryl halide phosphine section] Under nitrogen protection, 65 kilograms of yellow phosphorus is placed in a pressure-resistant reaction kettle, and 370 kg of chlorobenzene and 48 kg diphenyl phosphine are sequentially added from the automatic metering infusion tank. The mixture is closed itself. After the pressure conditions were heated to 370-395 degrees Celsius for 6 hours, the reaction system was cooled to room temperature, and the liquid phase mixture was directly automatically input to the distillation, and the hierarchical distillation device was opened, and the chlorobenzene and trichloride were first evaporated under normal pressure. The mixture of phosphorus (recovered), and the restriction rectification is sequentially collected to obtain 201 kg phenyl dichloride (recovery) and 242 kg of diphenylphosphine. [Aryl phenylphosphonate section] Under nitrogen protection, the 242 kg...

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Abstract

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.

Description

[Technical field][0001]The present invention relates to the field of new material chemicals in photocurable function, and a high-performance liquid phase flow line continuous automation production technology of a kind of acylphophosphine oxide organic phosphine compound is disclosed, which can produce a single-specific target product. The type of product mixture of two or more of the two or more. The process technology has highlighted low-cost economic competitiveness and environmentally friendly characteristics for large-scale manufacturing of target products. The target product includes average trimethylbenzoyl diphenyl oxide (also known as "2,4,6-trimethylbenzoyl diphenyl phosphine", trade name TPO) and average trimethylbenzene Formylphenylphosphonic acid ethyl ester (trade name TPO-L) and its structural analogs, and mixtures thereof. This type of organic phosphine compound is a widely used hydroken bond (C = C) unsaturated radiation polymerization system photosensitive initiator...

Claims

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Application Information

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IPC IPC(8): C07F9/32C07F9/40C07F9/53C07F9/572
CPCC07F9/3264C07F9/3288C07F9/4065C07F9/4075C07F9/5337C07F9/572Y02P20/54
Inventor 王智刚赵新阳丁浩宇
Owner SHENZHEN UV-CHEMTECH CO LTD
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