Purification method and application of 2, 2 '-biphenoxy phosphorus-chlorine compound

A technology of biphenoxy phosphorus chloride and purification method is applied in the field of chemical industry and can solve the problems of complex reaction system, low bisphosphite yield and the like

Pending Publication Date: 2021-03-12
CHINA NAT OFFSHORE OIL CORP +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the intermediates of this method have not been purified, the reaction system is relatively complicated, and the yield of bisphosphite is usually lo

Method used

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  • Purification method and application of 2, 2 '-biphenoxy phosphorus-chlorine compound
  • Purification method and application of 2, 2 '-biphenoxy phosphorus-chlorine compound
  • Purification method and application of 2, 2 '-biphenoxy phosphorus-chlorine compound

Examples

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Effect test

Embodiment 1

[0079] This example provides a purification method for 2,2'-biphenoxyphosphorous chloride compounds, including:

[0080] The 50L glass reactor was replaced with nitrogen three times, phosphorus trichloride (10.00kg) was added at 0°C, 2,2′-biphenol (8.04kg) was added in batches while stirring, and stirring was continued for 15 hours to 2, 2'-biphenol was completely dissolved. Then heat up to reflux and continue to react for about 3 hours, then add triethylamine (1.09kg), dichloromethane (4L), toluene (6L) mixed solution, control the temperature to 80°C and steam under normal pressure to distill out the mixture containing phosphorus trichloride and Distill the mixture of hydrogen chloride for about 3 hours until no liquid flows out; then increase the temperature to 115°C and change to vacuum distillation, keep the vacuum at 50mbar and continue distillation for 2 hours, stop the distillation and cool to room temperature, brown viscous residual liquid in the reaction kettle It ca...

Embodiment 2

[0086] This example provides a purification method for 2,2'-biphenoxyphosphorous chloride compounds, including:

[0087] The 50L glass reactor was replaced with nitrogen three times, phosphorus trichloride (10.00kg) was added at -10°C, 2,2′-biphenol (8.04kg) was added in batches while stirring, and stirring was continued for 12 hours to 2 , 2′-biphenol was completely dissolved. Then raise the temperature to reflux and continue the reaction for about 3 hours, then add pyridine (1.35kg), 1,1-dichloroethane (5L), and xylene (5L) mixed solution, control the temperature to 70°C and steam under normal pressure Distill the mixture of phosphorus chloride and hydrogen chloride for about 3 hours until no liquid flows out; then raise the temperature to 125°C for vacuum distillation, keep the vacuum at 20mbar and continue distillation for 1.5 hours, stop the distillation and cool to room temperature, the brown viscous The thick residue can be used as a raw material for the synthesis of b...

Embodiment 3

[0093] This example provides a purification method for 2,2'-biphenoxyphosphorous chloride compounds, including:

[0094] The 50L glass reactor was replaced with nitrogen three times, phosphorus trichloride (7.20kg) was added at -5°C, 2,2′-biphenol (8.04kg) was added in batches while stirring, and stirring was continued for 30 hours to 2 , 2′-biphenol was completely dissolved. Then raise the temperature to reflux and continue to react for about 3 hours, then add imidazole (0.92kg), dichloromethane (2.2L), xylene (2.8L) mixed solution, control the temperature to 75°C and distill out the phosphorus trichloride containing Distill the mixture of hydrogen chloride and hydrogen chloride for about 3 hours until no liquid flows out; then increase the temperature to 125°C and change to vacuum distillation, keep the vacuum at 10mbar and continue distillation for 1 hour, stop the distillation and cool to room temperature, brown sticky residue in the reaction kettle The solution can be us...

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Abstract

The invention provides a purification method and application of a 2, 2 '-biphenoxy phosphorus-chlorine compound, and the purification method comprises the following steps: after the reaction of a 2, 2'-biphenol compound and phosphorus trichloride is finished, adding a composition of organic amine and a mixed solvent to carry out program temperature control distillation purification to obtain the 2, 2 '-biphenoxy phosphorus-chlorine compound; the purification method can effectively reduce the concentration of residual hydrogen chloride, phosphorus trichloride and incompletely reacted aryloxy phosphorus dichloride in reactants, improves the yield and purity of the 2, 2 '-biphenoxy phosphorus-chlorine compound, can effectively improve the yield and purity of bisphosphite when being used in the synthesis of bisphosphite, can effectively reduce content of phosphorus impurities, acid and chloride ions in the bisphosphite is effectively reduced, and meets various requirements of industrial application control indexes.

Description

technical field [0001] The invention belongs to the technical field of chemistry and chemical engineering, and relates to a purification method and application of 2,2'-biphenoxyphosphorous chloride compounds. 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. For example, the catalytic system formed with metal rhodium in the oxo synthesis reaction has excellent catalytic activity and selectivity for olefin hydroformylation, and the synthesis of this compound has received great attention. [0003] In industrial production equipment, the carbonylation synthesis reaction has extremely high requirements on the purity and impurity content of bisphosphite. Phosphorus impurities, acids, chloride ions, etc. will all affect the reaction system, and phospho...

Claims

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Application Information

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IPC IPC(8): C07F9/6574
CPCC07F9/65744
Inventor 傅送保王兴永蒋志魁侯章贵胡先君王志军雷帅陈和柴文正
Owner CHINA NAT OFFSHORE OIL CORP
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