Preparation method of diphosphite

A bisphosphite and phosphorus trichloride technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve environmental protection, health and safety problems, and reaction operation steps cumbersome, easy to block the outlet pipe and other problems, to achieve the effect of safe and reliable reaction operation, fast mass transfer and heat transfer, avoiding environmental protection and health and safety

Active Publication Date: 2019-02-22
CHINA NAT OFFSHORE OIL CORP +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] However, in the existing disclosed technology, a large excess of phosphorus trichloride is used as a phosphating reagent, or a biphenoxyphosphorus chloride intermediate is obtained by vacuum distillation, or a catalyst is used to accelerate the reaction process, and excessive phosphorus trichloride and The hydrogen chloride produced in the reaction process is highly irritating and corrosive, and the reaction operation steps are cumbersome, which can easily cause environmental protection and health and safety problems; the vacuum distillation method requires extremely high temperature and vacuum, and the energy consumption in the production process is large; The use of catalysts to accelerate the reaction process will produce a large amount of aerosol white solid salt, which is very easy to block the outlet pipe

Method used

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  • Preparation method of diphosphite
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  • Preparation method of diphosphite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] The following structural formula is the synthesis of bisphosphite bis(2,2'-biphenol)-3,3',5,5'-tetra-tert-butyl-2,2'-biphenolate of the following formula III-1:

[0060]

[0061] (a) Dissolve phosphorus trichloride and pyridine in tetrahydrofuran in the premixer A1, control the concentration of phosphorus trichloride to be 1.5mol / L, and the concentration of pyridine to be 3.1mol / L, adjust the premixer by metering pump The flow rate of A1 is 10mL / min; 2,2'-biphenol is dissolved in tetrahydrofuran in the premixer A2, and the flow rate of the premixer A2 is adjusted to 10mL / min by a metering pump; The raw material is injected into the continuous flow reaction module F1 through a metering pump, keeping the temperature at 20°C, and the residence time is 10 minutes; then flows into the reaction module F2, keeping the temperature at 90°C, and the residence time is 8 minutes, and enters module B to cool after the reaction is completed.

[0062] (b) In premixer A3, dissolve 3...

Embodiment 2

[0066] The following structural formula is bisphosphite bis(2,2'-biphenol)-3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-biphenol of the following formula III-2 Synthesis of esters:

[0067]

[0068] (a) Dissolve phosphorus trichloride and pyridine in 2-methyltetrahydrofuran in the premixer A1, control the concentration of phosphorus trichloride to be 1.8mol / L, and the concentration of pyridine to be 3.8mol / L, through the metering pump Adjust the flow rate of premixer A1 to 12mL / min; dissolve 2,2'-biphenol in 2-methyltetrahydrofuran in premixer A2, and adjust the flow rate of premixer A2 to 12mL / min through a metering pump; Inject the raw materials in the above two premixers into the continuous flow reaction module F1 through the metering pump, keep the temperature at 15°C, and stay for 15 minutes; then flow into the reaction module F2, keep the temperature at 80°C, and stay for 10 minutes, and enter the module after the reaction B cools down.

[0069] (b) In premixer A3, 3,3'-d...

Embodiment 3

[0073] The following structural formula is the synthesis of bisphosphite bis(3,3'5,5'-tetra-tert-butyl-2,2'-biphenol)-2,2'-biphenolate of the following formula III-3:

[0074]

[0075] (a) Dissolve phosphorus trichloride and triethylamine in 2-methyltetrahydrofuran in premixer A1, control the concentration of phosphorus trichloride to be 1.2mol / L, and the concentration of triethylamine to be 2.5mol / L , adjust the flow rate of premixer A1 to 11mL / min through a metering pump; dissolve 3,3'5,5'-tetra-tert-butyl-2,2'-biphenol in 2-methyl In tetrahydrofuran, adjust the flow rate of the premixer A2 to 11mL / min through the metering pump; inject the raw materials in the above two premixers into the continuous flow reaction module F1 through the metering pump, keep the temperature at 20°C, and the residence time for 20min; then flow into the reaction In module F2, the temperature is maintained at 80°C, and the residence time is 15 minutes. After the reaction is completed, it enters ...

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Abstract

The invention discloses a preparation method of diphosphate. The method is characterized by mixing reaction raw materials based on agent dosage, and performing continuous flow micro-reaction to obtainthe diphosphate. According to the preparation method, the reaction process can be accurately controlled, and intermediate separation and exposing can be avoided, so that the risk of harmful substances to environmental protection and health safety can be avoided; in addition, the mass transferring and heat transferring are quick in the reaction process; little byproducts are produced; the reactionyield, the reaction purity and the reaction efficiency are extremely increased.

Description

technical field [0001] The present invention relates to the field of chemical synthesis. More specifically, it relates to a method for preparing bisphosphite. Background technique [0002] The molecular structure of the bisphosphite compound contains two coordinated phosphorus atoms, which can chelate with transition metals to form metal complexes. This compound plays an important role in various reactions catalyzed by transition metals. [0003] Some synthetic methods of bisphosphite compounds are disclosed in the prior art. For example, in one method, the first step is to react with excess phosphorus trichloride and 2,2-biphenol, and obtain biphenyl by vacuum distillation. In the second step, the biphenoxyphosphorus chloride intermediate and the substituted biphenol are reacted in triethylamine and dry toluene at minus 40°C, and finally washed with water, filtered and recrystallized to obtain bis Phosphite compounds. [0004] In yet another method, the first step reacts...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574
CPCC07F9/65746
Inventor 王兴永傅送保王凯侯章贵张卉雷帅
Owner CHINA NAT OFFSHORE OIL CORP
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