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Method for purifying organic diphosphite compound

A technology of organic diphosphite and diphosphite, which is applied in the field of purifying organic diphosphite compounds, can solve the problems that the possible application of diphosphite is not described, and achieve the effect of simple and effective method and content reduction

Active Publication Date: 2017-07-04
BASF SE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0036] US2003 / 0100787 describes a process for the preparation of sterically hindered triaryl monophosphites, but does not describe possible applications for the preparation of diphosphites

Method used

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  • Method for purifying organic diphosphite compound
  • Method for purifying organic diphosphite compound
  • Method for purifying organic diphosphite compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0276] Example 1: Using methylimidazole Hydrochloride as a catalyst for the synthesis of 6-chlorodibenzo[d,f][1,2,3]dioxaphosphine

[0277] Combine 2,2'-dihydroxybiphenyl (931.1g, 5.0mol) and 1-methylimidazole under nitrogen The hydrochloride (0.9g, 7.6mmol) was placed in a 2000ml double-walled reactor and heated to an internal temperature of 142°C after the 2,2'-dihydroxybiphenyl was melted. Then start to introduce phosphorus trichloride (861.2 g, 6.26 mol) while stirring to ensure that the phosphorus trichloride does not fall on the wall of the hot reactor. The introduction rate is adjusted so that the connected HCl scrubber absorbs all the HCl formed. Adding the phosphorus trichloride requires a total of 3 hours. After adding the phosphorus trichloride, the mixture was stirred for another 3 hours at 140°C to obtain a yellow fluid reaction mixture. The reactor was then evacuated to a final vacuum of 16 mbar within 40 minutes to remove excess phosphorus trichloride. The fin...

Embodiment 2

[0278] Example 2: Synthesis of 6-chlorodibenzo[d,f][1,3,2]dioxaphosphine using N-methylpyrrolidone as a catalyst

[0279] Under nitrogen, 2,2'-dihydroxybiphenyl (88.0kg, 473mol) and N- were added to a 600-liter vessel provided with an inclined blade stirrer, condenser, exhaust gas discharge device through the scrubber, and a vacuum generating device. Methylpyrrolidone (0.337kg, 3.4mol). The mixture was melted by heating to an internal temperature of 140°C and at this time phosphorus trichloride (88.5 kg, 644 mol) was introduced at 140°C in a total of 7 hours. The reaction is slightly endothermic under vigorous release of HCl and gentle reflux. After all the phosphorus trichloride was added, the mixture was stirred at 140°C for another 9 hours, and then cooled to a container internal temperature of 50°C. Then the vessel was slowly evacuated at 50°C to a final pressure of 20 mbar (condenser temperature 5°C) to remove excess phosphorus trichloride. Excess phosphorus trichloride i...

Embodiment 3

[0280] Example 3: 6,6'-[[3,3',5,5'-tetrakis(1,1-dimethylethyl)-1,1'-biphenyl]-2,2'-diyl ]Bis(oxy)]bis-dibenzo[d,f][1,3,2]dioxaphosphine

[0281] Mix 3,3',5,5'-tetrakis (1,1-dimethylethyl)-1,1'-biphenyl-2,2'-diol while stirring at 85℃ within 60 minutes (92.7kg) the solution in the mixture of 1-methylimidazole (40.8kg) and toluene (313.5kg) was added 6-chlorodibenzo[d,f][1,3,2] obtained according to Example 2 Dioxaphosphaheptine (118.4 kg) in the melt. At the end of the addition there were two phases and these were stirred for another hour at 80°C. Then the internal temperature was raised to 90°C, the stirrer was turned off to allow the phases to separate and the phases were allowed to stand still for 20 minutes at 90°C to separate. 1-methylimidazole as the lower phase Hydrochloride (59kg) and this crystallized immediately. Of the upper phase remaining in the container 31 P-NMR confirmed that it is 6,6'-[[3,3',5,5'-tetra(1,1-dimethylethyl)-1,1'-biphenyl]-2,2'- Diyl]bis(oxy)]b...

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Abstract

The invention relates to a method for purifying organic diphosphite compounds.

Description

[0001] Background of the invention [0002] The invention relates to a method for purifying an organic diphosphite compound. [0003] current technology [0004] Organic diphosphite compounds have a very wide range of applications, such as being used as chelating ligands in homogeneous catalysis, and also as flame retardants and UV stabilizers. It has been found that special rhodium complexes with organic diphosphite compounds can be used as catalysts for the hydroformylation of olefins because firstly they have high catalytic activity and secondly mainly result in linear aldehydes which are preferred for many applications. Organic diphosphite compounds are also suitable as hydrocyanation, hydrogenation, carbonylation, hydroacylation, hydroamidation, hydroesterification, hydrosilylation, hydroboration, alcoholysis, isomerization, allyl position Ligands of transition metal complex catalysts for alkylation or hydroalkylation. [0005] Such diphosphite compounds, their preparation and t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574
CPCC07F9/65746C07F9/65744
Inventor U·伯伦斯H·甘兹F·N·温德林W·埃尔-阿克达
Owner BASF SE
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